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A Office 3,049,554 Paiented Aug --a Office 3,049,554 Paiented Aug. 14, 1962 2 3,049,554 above. The preferred compounds of our invention are 9,1-D HALOGENG-320-D2 KETOPRESNANES AND the 9c, 11,3-difluoropregnenes and pregnadienes. The di PRO CESSES FOR THER EAANUEFACTURE flucro compounds of the general formula having a 17 c.21 David H. Gould, Leonia, and Hans Reinana, Siocrified, dihydroxy function and in particular a A1-bond are highly N.J., assignors to Sciering Corporation, Soon fied, potent agents useful in the treatment of inflammations, N.J., a corporation of New Jersey burns and atopic dermatoses. No Drawing. Filled Juae i, 1959, Ser. No. 837,843 in olir co-pending application Serial No. 743,492, filed 9 (Ciaias. (C. 269-397.3) ine 20, 1958, now U.S. Patent No. 2,894,963, of which this application is a continuation-in-part, we described This invention relates to a novel class of halogenated 0. 9,11-dihalcgeno-4-pregnene-170,21-diol-3,20-diones and steroids which are therapeutically useful. More specifi the corresponding 1,4-pregnadienes wherein the more elec cally, our invention relates to a particular group of 9,11 tronegative atom appeared at C-11 in the case wherein dihalogenated pregnanes wherein the halogen atom at C-9 the 9- and 11-substituent were different. Due to the limi is at least as electronegative as the halogen substituent at tations of the process described in said application, com C-11. By the term pregnane series we mean pregnanes polinds containing fluorine at C-9, or in the case of a containing the A-3,20-diketo and A.-3,20 diketo systems. mixed dihalide compound containing the more electro Our novel compounds are of the group consisting of negative atom at C-9, could not be prepared and were pregnanes having the following formula: specifically disclaimed. We have now found methods for CE.R. preparing such 9oz-fluoro compounds and compounds con taining the more electronegative halogen at C-9 as de -9 scribed by Formula i. Our novel compounds are prepared either from a A9(11). dehydro precursor or from a 9oz-halo-11-hydroxy pre r) cursor; the choice depending upon the halogen atoms to / 25 be present in the final product. k In order to prepare the difluoro compound of our in vention several routes are available. Starting with a o-\/\/ AC-pregnene such as 1,4,9011) - pregnatriene - 170,21 and the 1,2-dihydro analogs thereof, wherein R is a mem diol-3,20-dione 21-acetate and subjecting same to the ber of the group consisting of H, OH, and O-acyl, the acyl 30 action of a Suitable fluorinating agent there is obtained function being an acid radical of the group consisting of the 90,11.f3-difluoro analog. We have found agents such lower alkanoic acids having up to eight carbon atoms, as lead tetrafluoride, lead dioxide in conjunction with hy dibasic organic acids having up to eight carbon atoms, and drogen fluoride, iodosobenzene diacetate in conjunction phosphate; Z is a member of the group consisting of H, with hydrogen fluoride to be useful in effecting the trans OH and O-acyl, X and Y are halogen pairs of the group formation. Other fluorinating agents such as antimony consisting of (F, F), (F, Cl), (F, Br) and (Cl, Br) re pentafluoride, iodine heptafluoride, and bromine trifluo spectively, and the 2a-methyl, 6a-methyl, 16-lower alkyl ride also are useful. (c. or (3) analogs thereof. The reaction is usually carried out in an inert solvent Illustrative of the 21-esters falling within the foregoing at reduced temperatures, generally at -20° to -30° C. are lower alkanoates such as acetate, propionate, t-butyi 40 Representative of inert reactions solvents are chloroform, acetate, cyclopentyl propionate, and the like. Other esters methylene chloride, and tetrahydrofuran and the like. are prepared from dibasic organic acids such as succinate, Thus by our preferred method, 1,49(11)-pregnatriene phthalate, sulfobenzoate and the like. Representative of 170,21-diol-3,20-dicine 21-acetate is reacted with lead tet the 17-esters are acetate, propionate, caproate and the like. rafluoride in chloroform at -30° C. and there is ulti Curnovel compounds having the 1,4-pregnadiene-17,21 45 mately obtained 9a, 11g-difluoro-1,4-pregnadiene-17a,21 diol system are glucocorticoids useful in the treatment of diol-3,20-dione 21-acetate. inflammatory conditions. They are especially useful in Alternatively, the two halogen atoms may be introduced topical formulations such as creams or ointments. The in a sequence of two distinct reactions rather than through corresponding 1,2-dihydro analogs also exhibit these prop a simultaneous introduction. While this method is par erties but to a lesser extent and are more valuable as inter ticularly valuable for diheterohalogenation such as in pre mediates. paring a 9oz-fluoro-11p-chloropregnene, it is equally appli Those compounds of our invention which are devoid of cable to homohalogenation such as in preparing a 9a–116 oxygen at C-21 are active progestational agents which are difluoropregnene. By this route, a 96,11(3-oxidopregnene specific in their action and from which is absent andro is treated with hydrohalic acid and there is obtained the genic, estrogenic or corticoid activity. They are accord corresponding 9 cy-halo-11p-hydroxy compound. The halo ingly useful for conditions requiring progestational agents hydrin is subjected to one of several reaction sequences such as functional dysmenorrhea, premenstrual tension, described below whereby the 11,3-hydroxy function is re habitual or threatened abortion, and the maintenance of placed by the desired 11 (3-halogen group. pregnancy. In the direct replacement of an esterified 11-hydroxy Our novel compounds are essentially devoid of systemic 60 group an inversion of the configuration at C-11 appar mineralo effects such as salt retention. Thus our novel ently occurs. Thus, in order to obtain an 116-halogen via compounds, containing a 9a-fluoro group or 9a-chloro this route, it is necessary to start with an 11oz-hydroxy group-heretofore believed to be potent salt retention function. Starting with a 9oz-halogeno-1 16-hydroxy com factors are singularly devoid of such action and accord pound prepared as described above, the desired 9oz-halo ingly lend themselves to use in the conditions described geno-11&-hydroxy compound is obtained by oxidation to 3,049,554 3 4. the 11-keto function, as for example with chromic acid, Alternatively, the halogen at C-11 may be introduced followed by stereospecific reduction. The stereospecific through treatment of a 9oz-fluoro-11oz-amino-pregnane with reduction to the ox-configuration is preferably effected with a nitrosyl halide or of 9oz-fluoro-116-amino-pregnane with Sodium amalgam in alcohol and there is thus formed the an alkyl nitrite followed by a hydrohalic acid. The req 90-fluoro-110-hydroxy compound. Other reducing agents uisite 9c.-fluoro-11 (c. and (3)-amino-pregnanes are pre Such as lead-sodium alloys are also useful. pared for example as follows: To prevent reduction by the sodium amalgam and al Treatment of 9oz-fluorocortisone with formaldehyde as cohol of ketonic functions other than that at C-11, the described above yields 9oz-fluoro-17 (20),20C21)-bis 3- and 20-keto groups of a 3,11,20-triketonic pregnene are methylenedioxy-4-pregnene-3,11-dione which upon cata preferably protected prior to reduction. The C-3-keto O lytic reduction first with hydrogen and palladium catalyst group is preferably protected by reacting with ethylene in pyridine followed secondly with hydrogen and platinum glycol in the presence of acid catalyst to form the 3-ethyl catalyst affords 9oz-fluoro-17 (20).20(21)-bismethylenedi eneketal. In those compounds where the 17a,21-dihy oxypregnane-3-ol-11-one. This pregnanolone when treat droxy-20-keto corticoid side chain is present, treatment ed according ot the process analogous to that described in with formaldehyde in the presence of a strong acid, results 15 the copending application of Oliveto and Rausser, Serial in formation of the 17 (20),20C21)-bismethylenedioxy No. 657,030, is converted to the 11-oxime and the oxime function. In those compounds possessing only the 20 is then catalytically reduced to the two amino stereoiso keto or 17a-hydroxy-20-keto side chain, the 20-keto group mers, 9oz-fluoro-11c -amino-17a (20),20C21)-bismethylene is protected by formation of a 20-ethyleneketal concur dioxypregnane-3-ol and 9oz-fluoro-11p-amino-17 oz (20),20 rently to the formation of the 3-ethyleneketal. There is 20 (21)-bismethylenedioxypregnane-3-ol. These two epi thus obtained as a result a 3,20-bisethyleneketal. mers are separated by chromatography. Thus, 9oz-fluoro - 4 - pregnene-17a,21-diol-3,11,20-tri The 9oz-fluoro - 11c - aminopregnane is then treated one upon treatment with formaldehyde in the presence of with an appropriate nitrosyl halide, for example, nitrosyl p-toluenesulfonic, sulfuric, or hydrochloric acid yields 9a chloride, whereupon there is obtained 9oz-fluoro-11g fluoro-17 (20).20(21)-bismethylenedioxy - 4 - pregnene 25 chloro-17 c. (20).20(21)-bismethylenedioxypregnane - 21 3,11-dione. Further, treatment with ethylene glycol in ol. The identical compound is obtained by treatment of the presence of acid catalysts similar to those described the 116-amino epimer with an alkyl nitrite, such as ethyl above then yields 9 cy-fluoro-17 (20),20021)-bismethylene nitrite and hydrogen chloride. In both reactions a small dioxy-5-pregnene-11-one-3-ethyleneketal. amount of the 9a-fluoro-11c-chloropregnane is formed Similarly, 9oz-fluoro - 4 - pregnene-3,11,20-trione is 30 and is easily separated by chromatography.
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