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The Preparation and Cleavage of Some Organogermanium Compounds Clare William Gerow Iowa State College

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The Preparation and Cleavage of Some Organogermanium Compounds Clare William Gerow Iowa State College Iowa State University Capstones, Theses and Retrospective Theses and Dissertations Dissertations 1956 The preparation and cleavage of some organogermanium compounds Clare William Gerow Iowa State College Follow this and additional works at: https://lib.dr.iastate.edu/rtd Part of the Organic Chemistry Commons Recommended Citation Gerow, Clare William, "The preparation and cleavage of some organogermanium compounds " (1956). Retrospective Theses and Dissertations. 13676. https://lib.dr.iastate.edu/rtd/13676 This Dissertation is brought to you for free and open access by the Iowa State University Capstones, Theses and Dissertations at Iowa State University Digital Repository. It has been accepted for inclusion in Retrospective Theses and Dissertations by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. THE PREPARATION AND CLEAVAGE OF SOME ORGANOGERMANlUM C OMPOUNDS Clare lilliam Gerow /Vv A Dissertation Submitted to the Graduate Faculty In Partial Fulfillment of The Requirements for the Degree of DOCTOR OF PHILOSOPHY Major Subject: Organic Chemistry- Approved: Signature was redacted for privacy. In Change of Major Work Signature was redacted for privacy. Head of Major Department Signature was redacted for privacy. Dean of Gradua'te ColCollege Iowa State College 1956 UMI Number: DP12710 INFORMATION TO USERS The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleed-through, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. UMI UMI Microform DP12710 Copyright 2005 by ProQuest Information and Learning Company. All rights reserved. This microform edition is protected against unauthorized copying under Title 17, United States Code. ProQuest Information and Learning Company 300 North Zeeb Road P.O. Box 1346 Ann Arbor, Ml 48106-1346 li \ TABLE OF CONTENTS Page I. INTRODUCTION 1 II. HISTORICAL 3 A, Pbyelcal Properties 4 1. Melting point 6 2. Boiling point 11 3. Density and refractive index 14 B, Chemical Properties 19 1. Bonds to carbon 19 2. The Ge-G-e 'bond 2? 3. The hydrides 31 h. Bonds to oxygen 37 a. Germanols 37 b. Germanium oxides hZ c. Alkoxidee 48 d. Eeters ^1-9 5. Bonds to nitrogen 5^ 6, Bonds to halogens 60 C, Physiological Activity 68 III. EXPERIMEMTAL 9^ A. Preparation of Starting Materials 96 1. Tetrephenylgerinane 96 2. HexaphenyIdigermane 97 3. Triphenylbrofflogermane 98 5-. Triphenylchlorogermane 100 5. Triphenylgermane 101 B, Triphenylgermylmetallic Compounds 101 1. TriphenylgermylpotaBsium 101 Tl^l057 ill Page a. From he xap he nyl dl germane 101 (l) with tetrahydrofuran 102 Cil) with bromobenzene 102 (ill) In diethyl ether without initiator (attempted) 103 (Iv) With sodiuia-potaBSlum alloy in refluxing di-jgi-butyl ether (attempted) 103 (v) With eodluffl-potassium alloy in refluxing xylene (attempted) 104 (vi) With eodium-potaesium alloy in benzene (attempted) 104 (vii) With potaseium in refluxing xylene (attempted) I05 (viii) With Bodium-potaesium alloy in tetrahydrofuran (attempted) 106 (ix) With sodium-potaeeium alloy in ethylene glycol dimethyl ether (attempted) 106 (x) With potagsium in ethylene glycol dimethyl ether (G-BME) Tattempted) 107 b. From tetraphenylgermane IO7 ( i) In diethyl ether 10? (ii) In ethylene glycol dimethyl ether (GDME) 108 (iii) In benzene (attempted) 109 c. From triphenylbromogermane (attempted) 109 2. Triphe nylgermyllit hium 109 a. From tetraphenylgermane 109 b. From hexaphenyldigermane 111 c. From triphenylchlorogermane 111 C. Other Organogermylmetallic Compounds 112 1. Diphe ny1-2-phe nyle t hylge rmyllit hium 112 2. Triphenylgermylsodiiim (attempted) 113 a. From hexaphenyldigerm^ane 113 b. From triphenylgermane 113 iv Page 3. Triphenylgermyloeeiuni (attempted) 114 Triphenylgermylffiagneelum chloride (attempted) 114 5. Trlbenzylgermyllithlum (attempted) 115 6. Tri-n-butylgernyllithium (attempted) 116 7. Tri-n-hexylgeriayllithium (attempted) 116 8. Tri-n-oetylgerffiylllthiuffi (attempted) 117 9. Tri-n-btitylgermylpotasslum (attempted) 118 10, frlB-(2-phenylethyl)-germyllithlum (attempted) 119 11. TriethyIgermylllthium (attempted) 119 D. Preparation of Other Organogermanium Compounds 120 1. Tetrasubetituted germanee 120 a. friph@nyl-2-phenylethylgerfflane 120 b. Trlphenyl-3-phenylpropylgermane 121 c. Tripfoenylallylgermane 122 d. Tetra-n-hexylgermane 122 (i) From hexylaiagnsBium bromide 122 (il) From hexyllithlum 123 e. Trlphenyl-n-octadecylgermane 123 f. 1,l-Dlphenyl-2-triphenylgermylethane 124 2. Organogeraanes containing functional groupe 125 a. Ethyl trlphenylgermanecarboxylate (attempted) 125 (i) Direct eBterlfication 125 (li) Proffi tiiionyl chloride and acid 126 b. Triphenylchloromethylgermane 126 (i) From chloroiBethyltrlchlorogerinane 126 (11) Fro© triphenylhydroxymethyi- germane and thlonyl chloride (attempted) 127 c. Triphenylbromometiiylgermane (attempted) 127 d. Triphenyllodomethylgerinane (attempted) 128 V Page e. Trlphenyl-l-chloroethylgermane 128 f, Trlphenyl-2-chloropropylgermane (attempted) 129 g, Trlphenyl-alpha^broiaobenzylgermane 129 h. Triphenyl~2-bromo-2-phenyle thylgermane (attempted) 130 1, TrlphenylgermylBiethylmagneeium chloride I30 J, Trlphenylgermylmethyllithlum (attempted) 131 B. OrganogeManes Containing Another Group IV B Element 132 1, Preparation 132 a. Triphenylsilyltrlphenylgermane 132 b. Triphenylgermyltriphenyltln 133 0. Triphenylgermyltriphenyllead (attempted) 134 d. Triethylsilyltriphenylgermane 13^ e. 1-TriphenyIge rrayl-3-1r iphe ny1elly1- propane (attempted) 135 2. Reactions 135 a. Triphenylgermyltriphenylsilane 135 (1) With oxygen in refluxlng xylene 135 (11) With iodine in refluxlng chloro­ form 135 (ill) With Iodine In refluxlng xylene 136 (iv) With sodium-potasBlurn alloy 136 b. Triphenylgermyltriphenyltin 137 (i) With oxygen 137 (11) With iodine 137 (ill) ¥lth sodium-potaselum alloy 138 (iv) With phenyllithlusa 139 F. Reactions of Trlphenylgermylmetalllc Compounds 140 1, Trlphenylgerraylpotassluni 140 a. With _2-bromotoluene l4l b. With benzyl chloride l4l vl Page c. With trane-etilbene 1^1 d. With 1,1-diphenylethylene 1^2 e. With benzophenone 1^2 2. TrlphenylgeriBylllthlun! 1^3 a. halides (i) Methyl iodide (11) Ethyl bromide IM (ill) Trlethylchlorosilane 144 (iv) Phenacyl chloride 145 b. ^Ith olefins 145 (1) trang-Stllbene 145 (11) l,l~Dlphenylethylene 145 (ill) Octadecene-1 146 (iv) Octene-1 147 (y) Cyclohexene 148 (vl) Benzalacetophenone l48 c. nth other compoundB containing unsaturated linkages 149 (i) Benzophenone anil 149 (11) Benzalanillne 150 (ill) Benzonltrile 150 (iv) Pyridine 150 (v) Qulnollne 151 (vl) Azobenzene 151 (vil) Azoxybenzene 151 (vlli) Acetaldehyde 152 (ix) Benzaldehyde 153 (x) ^-Eenzoqulnone 153 d. With mlscellaneouB compounds 154 (1) With fluorene 154 (11) With dlbenzofuran 155 (ill) 1/^lth bromine 155 e. With epoxides 156 Til Page (i) Ethylene oxide 156 Cil) Propylene oxid® 157 (ill) Styrene oxide 157 &. Reactione of Triphenylgermane 158 1. With olefins 158 a» Octadecene-1 158 b. Triphenylellylgermane 159 2. With organollthlum reagents 159 a. Methyllithluia 159 (l) At room temperature 159 (il) In refluxlng ether 160 b. Butylllthium 161 c. Triphenylgermylllthlum 161 H. Thermal Stabilities of Organogermanlum Compounds 163a IV. DISCUSSION 165 A. Trlphenylgermylffietalllc Compounde 165 B. Compounds Containing Germanium and Another Group IV B Element 181 C. Triphenylgermane 183 D. Thermal Stability 188 ?. smmAm 189 VI. LITERATORE CITED 192 A. G-ermanlum References 192 B, Other References 200 VII. ACKNOWLEDGMENT 206 1 I. IHTRODUCTION Ever since Winkler (150) In 1887 reported the first organogermanium compound, tetraethylgermane, the primary method for the preparation of tetrasubetituted germanee has been the coupling of a reactive organoraetalllc reagent vith a germanluffl halide. In 192? Kraue (80) introduced triphenyl- germy Is odium and in 1932 (79) trlethylgerHiylpotassium as reagents for the preparation of organogermanium compounds, howver, he did not Investigate fully the potentialities of these reagents. The preparation of organohalogermanee by the direct reaction of hydrocarbon halides with elemental germani­ um in the presence of a catalyst was Introduced by Rochow (109) in 19^7. It has been the purpose of these Investigations to find new methode of introducing germanium into organic compounds In order that these compounds may be examined concerning their relationship to analogous silicon compounde and their thermal stability. This goal ifae achieved by the preparations of tri- phenylgermylpotaeslum and trlphenylgermylllthlum and the sub­ sequent Investigation of the reactions of these reagents with organic compounds to obtain compounde having high thermal stability or compounds containing functional groups capable of being operated upon to obtain a different product 2 exMMtlng the desired qualities. It has been found that both triphenylgermylpotaesium &na trlphenylgerffiylllthlum poes@is & degree of reaotlTity sufficient to react with olefins, carbonyl groups, azo and azomethine linkages, epoxides and halides., thus enabling one to synthesize a Tsrlety of org&nogeriBaniuffl compounde. 3 II. HISfORIGAL 11 though there has been a treicencloug amount of work re­ ported
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