Guidelines for Pyrophoric Materials
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Phosphorus Specialties: the cornerstone of synthesis for pharmaceutical applications Eamonn Conrad, Ph.D., Global BD Manager Dino Amoroso, Ph.D., NA Account Manager William Stibbs, Ph.D. Senior BD Manager Overview • Solvay Phosphorus Specialties, Strem Chemicals Inc. Partnership • Chemistry for the Manufacture of Phosphine Ligands • Applications in Pharmaceutical Catalysis • Applications in Life Sciences • Summary and Questions *Solvay partners with Strem Chemicals for sample distribution page 2 Phosphorus Specialties Strem Chemicals, Inc. Solvay partners with Strem Chemicals for sample distribution! Established in 1964 More than 55 years of experience in manufacturing and handling high quality inorganics and organometallics 5,000+ specialty chemicals available Laboratory Chemicals for R&D cGMP Products Manufactured in Kilo-lab Suites High Pressure Materials Custom Synthesis Projects Customers include: Corporate Headquarters Academic, industrial and government R&D laboratories Corporate Headquarters European Headquarters Commercial scale businesses in the pharmaceutical, Newburyport, MA USA Strasbourg, France microelectronics, chemical & petrochemical industries Phosphorus Specialties Samples available from Strem Who We Are Phosphorus Specialties Mining Solutions Polymer Additives Putting our science to work for customers to develop differentiated products and technologies Dedicated on-site technical service and applications expertise to support our customers’ needs Deep customer relationships and ongoing collaborations to solve demanding -
Ep 2508506 A1
(19) & (11) EP 2 508 506 A1 (12) EUROPEAN PATENT APPLICATION (43) Date of publication: (51) Int Cl.: 10.10.2012 Bulletin 2012/41 C07C 67/343 (2006.01) C07C 227/08 (2006.01) C07F 5/02 (2006.01) C07C 229/34 (2006.01) (21) Application number: 11161611.6 (22) Date of filing: 08.04.2011 (84) Designated Contracting States: (72) Inventor: The designation of the inventor has not AL AT BE BG CH CY CZ DE DK EE ES FI FR GB yet been filed GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR (74) Representative: Kunic Tesovic, Barbara Designated Extension States: Lek Pharmaceuticals d.d. BA ME Sandoz Development Center Slovenia - Patents Verovskova 57 (71) Applicant: LEK Pharmaceuticals d.d. 1526 Ljubljana (SI) 1526 Ljubljana (SI) (54) Preparation of sitagliptin intermediates (57) The invention relates to the preparation of chiral compounds, in particular to the preparation of chiral compounds which may be used as intermediates for the preparation of anti-diabetic agents, preferably sitagliptin. EP 2 508 506 A1 Printed by Jouve, 75001 PARIS (FR) EP 2 508 506 A1 Description Field of the Intention 5 [0001] The present invention relates to the preparation of chiral compounds, in particular to the preparation of chiral compounds which may be used as intermediates for the preparation of anti-diabetic agents, preferably sitagliptin. Background prior art 10 [0002] Type II diabetes mellitus (T2DM) is a global epidemic. Therefore, the research is oriented in the development of selective inhibitors of the enzyme DPP-IV as a promising new treatment for the type II diabetes. -
Inorganic Syntheses
INORGANIC SYNTHESES Volume 27 .................... ................ Board of Directors JOHN P. FACKLER, JR. Texas A&M University BODlE E. DOUGLAS University of Pittsburgh SMITH L. HOLT, JR. Oklahoma State Uniuersity JAY H. WORRELL University of South Florida RUSSELL N. GRIMES University of Virginia ROBERT J. ANGELIC1 Iowa State University Future Volumes 28 ROBERT J. ANGELIC1 Iowa State University 29 RUSSELL N. GRIMES University of Virginia 30 LEONARD V. INTERRANTE Rensselaer Polytechnic Institute 31 ALLEN H. COWLEY University of Texas, Austin 32 MARCETTA Y. DARENSBOURG Texas A&M University International Associates MARTIN A. BENNETT Australian National University, Canberra FAUSTO CALDERAZZO University of Pisa E. 0. FISCHER Technical University. Munich JACK LEWIS Cambridge University LAMBERTO MALATESTA University of Milan RENE POILBLANC University of Toulouse HERBERT W. ROESKY University of Gottingen F. G. A. STONE University of Bristol GEOFFREY WILKINSON Imperial College of Science and Technology. London AKlO YAMAMOTO Tokyo Institute 01 Technology. Yokohama Editor-in-Chief ALVIN P. GINSBERG INORGANIC SYNTHESES Volume 27 A Wiley-Interscience Publication JOHN WILEY & SONS New York Chichester Brisbane Toronto Singapore A NOTE TO THE READER This book has been electronically reproduced from digital idormation stored at John Wiley h Sons, Inc. We are phased that the use of this new technology will enable us to keep works of enduring scholarly value in print as long as there is a reasonable demand for them. The content of this book is identical to previous printings. Published by John Wiley & Sons, Inc. Copyright $? 1990 Inorganic Syntheses, Inc. All rights reserved. Published simultaneously in Canada. Reproduction or translation of any part of this work beyond that permitted by Section 107 or 108 of the 1976 United States Copyright Act without the permission of the copyright owner is unlawful. -
Pyrophoric Materials
Appendix A PYROPHORIC MATERIALS Pyrophoric materials react with air, or with moisture in air. Typical reactions which occur are oxidation and hydrolysis, and the heat generated by the reactions may ignite the chemical. In some cases, these reactions liberate flammable gases which makes ignition a certainty and explosion a real possibility. Examples of pyrophoric materials are shown below. (List may not be complete) (a) Pyrophoric alkyl metals and derivatives Groups Dodecacarbonyltetracobalt Silver sulphide Dialkytzincs Dodecacarbonyltriiron Sodium disulphide Diplumbanes Hexacarbonylchromium Sodium polysulphide Trialkylaluminiums Hexacarbonylmolybdenum Sodium sulphide Trialkylbismuths Hexacarbonyltungsten Tin (II) sulphide Nonacarbonyldiiron Tin (IV) sulphide Compounds Octacarbonyldicobalt Titanium (IV) sulphide Bis-dimethylstibinyl oxide Pentacarbonyliron Uranium (IV) sulphide Bis(dimethylthallium) acetylide Tetracarbonylnickel Butyllithium (e) Pyrophoric alkyl non-metals Diethylberyllium (c) Pyrophoric metals (finely divided state) Bis-(dibutylborino) acetylene Bis-dimethylarsinyl oxide Diethylcadmium Caesium Rubidium Bis-dimethylarsinyl sulphide Diethylmagnesium Calcium Sodium Bis-trimethylsilyl oxide Diethylzinc Cerium Tantalum Dibutyl-3-methyl-3-buten-1-Yniborane Diisopropylberyllium Chromium Thorium Diethoxydimethylsilane Dimethylberyllium Cobalt Titanium Diethylmethylphosphine Dimethylbismuth chloride Hafnium Uranium Ethyldimthylphosphine Dimethylcadmium Iridium Zirconium Tetraethyldiarsine Dimethylmagnesium Iron Tetramethyldiarsine -
Download The
COORDINATION COMPOUNDS OF ALKYL GALLIUM HYDRIDES by VICTOR GRAHAM WIEBE B.Sc. (Hons.) University of British Columbia 1966 A THESIS SUBMITTED IN PARTIAL FULFILMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF SCIENCE In The Department of Chemistry We accept this thesis as conforming to the required standard The University of British Columbia June 1968 In presenting this thesis in partial fulfilment of the requirements for an advanced degree at the University of British Columbia, I agree that the Library shall make it freely available for reference and Study. I further agree that permission for extensive copying of this thesis for scholarly purposes may be granted by the Head of my Department or by hits representatives. It is understood that copying or publication of this thesis for financial gain shall not be allowed without my written permission. Department of The University of British Columbia Vancouver 8, Canada - ii - Abstract Although the organo hydride derivatives of boron and aluminum are well characterized^little work has been reported on the corresponding gallium systems. The present study was initiated to determine the relative stabilities and reactivity of organo gallium hydride derivatives as compared with the stabilities and reactions of the corresponding compounds of boron and aluminum. Various preparative routes to this new class of gallium compounds have been investigated. These include the use of organo-mercury, organo-lithium and lithium hydride derivatives in reactions with gallium hydride and gallium alkyl compounds and their halogen substituted derivatives: Me3NGaH3 + HgR2 >- Me3NGaH2R + l/2Hg + 1/2H2 Me3NGaH2Cl + LiR y Me3NGaH2R + LiCl Me3NGaR2Cl + LiH • Me3NGaHR2 + LiCl A fourth preparative method involves disproportionation reactions between gallium hydride compounds and organo gallium compounds to yield the mixed organo hydride derivatives. -
Phosphine-Catalyzed Additions of Nucleophiles and Electrophiles to Α
PHOSPHINE-CATALYZED ADDITIONS OF NUCLEOPHILES AND ELECTROPHILES TO α,β–UNSATURATED CARBONYL COMPOUNDS Reported by Michael Scott Bultman November 4, 2004 INTRODUCTION Organophosphorous compounds are becoming increasingly important in organic synthesis. Phosphines serve as precursors to phosphonium ylides in the Wittig reaction,1 and as nucleophilic triggers in the Mitsunobu2 and Staudinger3 reactions. In these processes, the phosphine is stoichiometrically consumed and converted into a phosphine oxide. Phosphines are also commonly used as ligands for transition metal-catalyzed reactions, to modulate reactivity and stereocontrol.4 On the other hand, the use of phosphines as nucleophilic catalysts for organic reactions has only gained attention in the last ten years. First reported by Rauhut and Currier in 1963,5 phosphine catalysis has since been reinvestigated after the phosphine ligands in some transition-metal-catalyzed reactions were found to be better catalysts than the metal/phosphine complexes alone!6 Phosphines are well suited for catalyzing the addition of both nucleophiles and electrophiles to electron deficient alkenes, alkynes, and allenes. Activation of these α,β-unsaturated carbonyl systems with the phosphine enables the formation of new bonds at the α-, β-, and γ-positions. This report will highlight these different modes of addition to α,β-unsaturated carbonyl systems under phosphine catalysis that allow for the formation of a wide array of products from a single class of substrates. GENERAL REACTIVITY OF PHOSPHINES Key characteristics required for successful nucleophilic catalysis lie in the balance of leaving group ability, nucleophilicity, and ease of ylid formation. Increasing leaving group ability can often be + correlated with decreasing basicity. -
Bond Formation Reactions to Phosphorus Using an Electrophilic Phosphinidene Complex
BOND FORMATION REACTIONS TO PHOSPHORUS USING AN ELECTROPHILIC PHOSPHINIDENE COMPLEX A Thesis Submitted to the Faculty of Graduate Studies and Research In Partial Fulfillment of the Requirements For the Degree of Doctor of Philosophy in Chemistry University of Regina By Kandasamy Vaheesar Regina, Saskatchewan September, 2013 Copyright 2013: K. Vaheesar UNIVERSITY OF REGINA FACULTY OF GRADUATE STUDIES AND RESEARCH SUPERVISORY AND EXAMINING COMMITTEE Kandasamy Vaheesar, candidate for the degree of Doctor of Philosophy in Chemistry, has presented a thesis titled, Bond Formation Reactions to Phosphorus Using an Electrophilic Phosphinidene Complex, in an oral examination held on August 28, 2013. The following committee members have found the thesis acceptable in form and content, and that the candidate demonstrated satisfactory knowledge of the subject material. External Examiner: *Dr. Stephen Foley, University of Saskatchewan Supervisor: Dr. Brian Sterenberg, Department of Chemistry/Biochemistry Committee Member: Dr. Mauricio Barbi, Department of Physics Committee Member: Dr. Allan East, Department of Chemistry/Biochemistry Committee Member: Dr. R. Scott Murphy, Department of Chemistry/Biochemistry Chair of Defense: Dr. Dongyan Blachford, Faculty of Graduate Studies & Research *Participated via Video Conference ABSTRACT Electrophilic phosphinidene complexes play a central role in organophosphorus chemistry. The chemistry of transient phosphinidene complexes has been well studied, but stable, cationic phosphinidene complexes are not as well understood. Therefore the i + 5 reactivity of a cationic phosphinidene complex [CpFe(CO)2{PN Pr2}] (Cp = η - cyclopentadienyl, iPr = isopropyl), toward bond activation, cycloaddition and nucleophilic addition has been examined. i + The complex [CpFe(CO)2{PN Pr2}] reacts with primary, secondary, and tertiary i + silanes to form the silyl phosphine complexes [CpFe(CO)2{P(H)(SiR3)N Pr2}] (SiR3 = SiPhH2, SiPh2H, Si(C2H5)3), in which the phosphinidene has inserted into the Si-H bond. -
List of Reactive Chemicals
LIST OF REACTIVE CHEMICALS Chemical Prefix Chemical Name Reactive Reactive Reactive CAS# Chemical Chemical Chemical Stimulus 1 Stimulus 2 Stimulus 3 111-90-0 "CARBITOL" SOLVENT D 111-15-9 "CELLOSOLVE" ACETATE D 110-80-5 "CELLOSOLVE" SOLVENT D 2- (2,4,6-TRINITROPHENYL)ETHYL ACETATE (1% IN ACETONE & BENZENE S 12427-38-2 AAMANGAN W 88-85-7 AATOX S 40487-42-1 AC 92553 S 105-57-7 ACETAL D 75-07-0 ACETALDEHYDE D 105-57-7 ACETALDEHYDE, DIETHYL ACETAL D 108-05-4 ACETIC ACID ETHENYL ESTER D 108-05-4 ACETIC ACID VINYL ESTER D 75-07-0 ACETIC ALDEHYDE D 101-25-7 ACETO DNPT T 126-84-1 ACETONE DIETHYL ACETAL D 108-05-4 ACETOXYETHYLENE D 108-05-4 1- ACETOXYETHYLENE D 37187-22-7 ACETYL ACETONE PEROXIDE, <=32% AS A PASTE T 37187-22-7 ACETYL ACETONE PEROXIDE, <=42% T 37187-22-7 ACETYL ACETONE PEROXIDE, >42% T S 644-31-5 ACETYL BENZOYL PEROXIDE (SOLID OR MORE THAN 45% IN SOLUTION) T S 644-31-5 ACETYL BENZOYL PEROXIDE, <=45% T 506-96-7 ACETYL BROMIDE W 75-36-5 ACETYL CHLORIDE W ACETYL CYCLOHEXANE SULFONYL PEROXIDE (>82% WITH <12% WATER) T S 3179-56-4 ACETYL CYCLOHEXANE SULFONYL PEROXIDE, <=32% T 3179-56-4 ACETYL CYCLOHEXANE SULFONYL PEROXIDE, <=82% T 674-82-8 ACETYL KETENE (POISON INHALATION HAZARD) D 110-22-5 ACETYL PEROXIDE, <=27% T 110-22-5 ACETYL PEROXIDE, SOLID, OR MORE THAN 27% IN SOLUTION T S 927-86-6 ACETYLCHOLINE PERCHLORATE O S 74-86-2 ACETYLENE D 74-86-2 ACETYLENE (LIQUID) D ACETYLENE SILVER NITRATE D 107-02-08 ACRALDEHYDE (POISON INHALATION HAZARD) D 79-10-7 ACROLEIC ACID D 107-02-08 ACROLEIN, INHIBITED (POISON INHALATION HAZARD) D 107-02-08 ACRYLALDEHYDE (POISON INHALATION HAZARD) D 79-10-7 ACRYLIC ACID D 141-32-2 ACRYLIC ACID BUTYL ESTER D 140-88-5 ACRYLIC ACID ETHYL ESTER D 96-33-3 ACRYLIC ACID METHYL ESTER D Stimulus - Stimuli is the thermal, physical or chemical input needed to induce a hazardous reaction. -
The Preparation of Organomagnesium Fluorides
THE PREPARATION OF ORGANOMAGNESIUM FLUORIDES BY ORGANOMETALLIC EXCHANGE REACTIONS AND THE COMPOSITION IN SOLUTION OF ALKOXY(METHYL)MAGNESIUM AND DIALKYLAMINO(METHYL)MAGNESIUM COMPOUNDS A THESIS Presented To The Faculty of the Graduate Division by John A. Nackashi In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy In the School of Chemistry Georgia Institute of Technology May, 1974 THE PREPARATION OF ORGANOMAGNESIUM FLUORIDES BY ORGANOMETALLIC EXCHANGE REACTIONS AND THE COMPOSITION IN SOLUTION OF ALKOXY(METHYL)MAGNESIUM AND DIALKYLAMINO(METHYL)MAGNESIUM COMPOUNDS Approved: E. C. Ashby, Chairman A. Bertrand C. L. Liotta Date approved by Chairman: ii ACKNOWLEDGMENTS The author is grateful to Dr. E. C. Ashby for his guidance, direction and patience during this research. The reading of this thesis by Dr. A. Bertrand and Dr. C. Liotta is greatly appreciated. The author is also indebted to John P. Oliver for his assistance and friendship, and to the mem bers of the research group who made the successes of this research a joy and the failures acceptable. The warm friend ship expressed by the research group will always be cherished. Financial assistance by the Georgia Institute of Tech nology and the National Science Foundation is gratefully ack nowledged. The author acknowledges a special appreciation to his parents and particularly his wife, Bryan. Their gentle en couragement and patient understanding throughout the entire period of study has made this thesis possible. iii TABLE OF CONTENTS Page ACKNOWLEDGMENTS ii LIST OF TABLES vi LIST OF ASSOCIATION PLOTS iii LIST OF SPECTRA ix SUMMARY x PART I THE PREPARATION OF ORGANOMAGNESIUM FLUORIDES BY ORGANOMETALLIC EXCHANGE REACTIONS CHAPTER I. -
Advanced Studies on the Synthesis of Organophosphorus Compounds
ALMA MATER STUDIORUM UNIVERSITÀ DI BOLOGNA DOTTORATO DI RICERCA IN SCIENZE CHIMICHE (XIX° ciclo) Area 03 Scienze Chimiche-CHIM/06 Chimica Organica Dipartimento di Chimica Organica “A. Mangini” Coordinatore: Chiar.mo Prof. Vincenzo Balzani Advanced Studies on the Synthesis of Organophosphorus Compounds Dissertazione Finale Presentata da: Relatore: Dott. ssa Marzia Mazzacurati Prof. Graziano Baccolini Co-relatore: Dott.ssa Carla Boga INDEX Index: Keywords…………………………………………………………….………….VII Chapter 1…………………………………………………………………………..3 GENERAL INTRODUCTION ON PHOSPHORUS CHEMISTRY 1.1 Organophosphorus Chemistry………………………………………………….4 1.1.1 Phosphines………………………………………………………………..5 1.1.2 Phosphonates……………………………………………………………..6 1.1.3 Phosphites………………………………………………………………...7 1.2 Uses of Organophosphorus Compounds………………………………………..7 1.2.1 Agricultural Application………………………………………………….8 1.2.2 Catalysis……………………………………………………………..…....9 1.2.3 Organophosphorus Conpounds in Medicine…………………………….11 1.2.4 Phosphorus in Biological Compounds…………………………………..12 1.3 References……………………………………………………………………..15 Chapter 2…………………………………………………………………………17 THE HYPERCOORDINATE STATES OF PHOSPHORUS 2.1 The 5-Coordinate State of Phosphorus……………………………………….17 2.2 Pentacoordinated structures and their non rigid character…………………….18 2.3 Permutational isomerization…………………………………………………..19 2.3.1 Berry pseudorotation……………………………………………………20 2.3.2 Turnstile rotation………………………………………………………..21 2.4 The 6-Coordinate State of Phosphorus……………………………………….22 2.5 References…………………………………………………………………......24 I Chapter -
Improved Processes for the Preparation of 1-Aryl-5-Alkyl Pyrazole Compounds
(19) TZZ¥__Z_T (11) EP 3 184 510 A1 (12) EUROPEAN PATENT APPLICATION (43) Date of publication: (51) Int Cl.: 28.06.2017 Bulletin 2017/26 C07D 231/18 (2006.01) (21) Application number: 16199220.1 (22) Date of filing: 22.04.2013 (84) Designated Contracting States: • LEE, Hyoung, Ik AL AT BE BG CH CY CZ DE DK EE ES FI FR GB Cary, NC 27519 (US) GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO • ZHAN, Xinxi PL PT RO RS SE SI SK SM TR BDA, Beijing 100176 (CN) Designated Extension States: • LABROSSE, Jean-Robert BA ME F-34160 Saint Hilaire De Beauvoir (FR) • MULHAUSER, Michel (30) Priority: 20.04.2012 US 201261635969 P F-69370 Saint Didier au Mont d’Or (FR) (62) Document number(s) of the earlier application(s) in (74) Representative: D Young & Co LLP accordance with Art. 76 EPC: 120 Holborn 13720198.4 / 2 852 577 London EC1N 2DY (GB) (71) Applicant: Merial, Inc. Remarks: Georgia 30096 (US) •This application was filed on 16-11-2016 as a divisional application to the application mentioned (72) Inventors: under INID code 62. • MENG, Charles, Q •Claims filed after the date of filing of the Grayson, GA 30017 (US) application/dateof receipt of the divisional application • LE HIR DE FALLOIS, Loic, Patrick (Rule 68(4) EPC). Atlanta, Georgia 30305 (US) (54) IMPROVED PROCESSES FOR THE PREPARATION OF 1-ARYL-5-ALKYL PYRAZOLE COMPOUNDS (57) Provided are improved processes for the preparation of 1-aryl pyrazole compounds of formula (I) and (IB): which are substituted at the 5-position of the pyrazole ring with a carbon-linked functional group. -
New Boron–Hydrogen Insertion Reactions of Ligated Boranes By
New Boron–Hydrogen Insertion Reactions of Ligated Boranes by Thomas H. Allen B.S. Chemistry, Magna Cum Laude, Ohio Northern University, 2012 Submitted to the Graduate Faculty of the Kenneth P. Dietrich School of Arts and Sciences in partial fulfillment of the requirements for the degree of Doctor of Philosophy University of Pittsburgh 2018 UNIVERSITY OF PITTSBURGH KENNETH P. DIETRICH SCHOOL OF ARTS AND SCIENCES This dissertation was presented by Thomas H. Allen It was defended on July 17, 2018 and approved by Sruti Shiva, Associate Professor, Department of Pharmacology and Chemical Biology W. Seth Horne, Associate Professor, Department of Chemistry Kay M. Brummond, Professor, Department of Chemistry Committee Chair: Dennis P. Curran, Distinguished Service Professor and Bayer Professor, Department of Chemistry ii Copyright © by Thomas H. Allen 2018 iii New Boron–Hydrogen Insertion Reactions of Ligated Boranes Thomas H. Allen, PhD University of Pittsburgh, 2018 Chemical transformations of ligated borane complexes, including N-heterocyclic carbene boranes, are demonstrated. Chapter 1 begins with an introduction of Lewis base borane complexes, rhodium carbene chemistry, and B–H insertion of ligated boranes. The second part of Chapter 1 describes the insertion of rhodium carbenes, previously demonstrated with NHC- boranes, into the B–H bonds of other ligated boranes. Stable ligated α-boryl esters were isolated. A series of competitive B–H insertion experiments are described that were used to develop a relative reactivity profile of ligated boranes toward rhodium-catalyzed B–H insertion. The enantioselective B–H insertion of NHC-boranes with chiral dirhodium catalysts was also investigated. Finally, the synthesis and application of two chiral bridged dirhodium catalysts is described.