GB843213A - Process for the production of pregnadienes - Google Patents

Process for the production of pregnadienes

Info

Publication number
GB843213A
GB843213A GB5071/57A GB507157A GB843213A GB 843213 A GB843213 A GB 843213A GB 5071/57 A GB5071/57 A GB 5071/57A GB 507157 A GB507157 A GB 507157A GB 843213 A GB843213 A GB 843213A
Authority
GB
United Kingdom
Prior art keywords
acetate
dione
pregnane
triol
diol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB5071/57A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Merck Sharp and Dohme Corp
Original Assignee
Schering Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Schering Corp filed Critical Schering Corp
Publication of GB843213A publication Critical patent/GB843213A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J5/00Normal steroids containing carbon, hydrogen, halogen or oxygen, substituted in position 17 beta by a chain of two carbon atoms, e.g. pregnane and substituted in position 21 by only one singly bound oxygen atom, i.e. only one oxygen bound to position 21 by a single bond
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J75/00Processes for the preparation of steroids in general

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Steroid Compounds (AREA)

Abstract

Cyclopentanophenanthrene compounds of the general formula: <FORM:0843213/IV(b)/1> wherein R represents hydrogen or an acyl group and X represents <FORM:0843213/IV(b)/2> are prepared by di-dehydrohalogenating a normal or allo-pregnane-2,4-dibromo-11X-17 a -ol 21-OR-3,20-dione, wherein R and X have the above significance, with a dehydrobrominating agent. The above process may be modified in that the 2,4-dibromo reactant is prepared by brominating a normal or allo-pregnane of the formula: <FORM:0843213/IV(b)/3> wherein R and X have the above significance. The acyl group is preferably the formyl group or an alkanoyl group having not more than 8 carbon atoms such as the acetyl, propionyl, butyryl or valeryl groups. The 21-ester group in the resulting 1,4-pregnadiene may be hydrolysed to form the corresponding free 21-hydroxy compound with an acid or base. The di-dehydrohalogenation step may be carried out by refluxing with collidine, quinaldine or dimethylaniline. The 21-esters of 11 a -hydroxy-pregnadienes of the above general formula may be prepared in a similar manner and then the 11 a - or 11BETA-hydroxy 1,4-pregnadienes may be oxidised to the corresponding 11-keto-1,4-pregnadienes, and, if required, hydrolysed to the corresponding 21-hydroxy compounds. The hydrolysis of the 21-ester group may be carried out before the oxidation of the 11 a - or 11b -hydroxy group. The bromination is preferably carried out in acetic acid or other inert organic solvent. The hydrolysis of the 21-ester group may be hydrolysed with an alkali metal base such as a carbonate, bicarbonate or hydroxide, in a solvent such as methyl or ethyl alcohol. In the examples:-(1) allopregnane-and pregnane-17 a ,21-diol-3,11,20-trione 21-acetate are brominated to form the corresponding 2,4-dibromo compounds and are didehydrobrominated to form 1,4-pregnadiene-17 a , 21-diol-3,11,20-trione 21-acetate; the 21-acetate is then hydrolysed to the corresponding 21-hydroxy compound; (2) allopregnane- and pregnane-11b ,17 a ,21-triol-3,20-dione 21-acetate are brominated to form the corresponding 2,4-dibromo compounds and are then di-dehydrobrominated to form 1,4-pregnadiene-11b ,17 a ,21-triol-3,20-dione 21-acetate; the 21-acetate is then hydrolysed to the corresponding 21-hydroxy compound; (3) pregnane-11 a ,-17 a ,21,triol-3,20-dione 21-acetate is brominated to form 2,4-dibromopregnane-11 a , 17 a ,21-triol-3,20-dione 21-acetate, the 2,4-dibromo compound is di-dehydrobrominated to form 1,4-pregnadiene-11 a ,-17 a ,21-triol-3,20-dione 21-acetate and hydrolysed to the corresponding 21-hydroxy compound, and the 21-hydroxy and the 21-acetate compound are then oxidised with chromium trioxide, N-bromacetamide or N-bromo-succinimide to form 1,4-pregnadiene-17 a ,21-diol-3,11,20-trione and the 21-acetate thereof respectively; (4) pregnane-17 a ,21-diol-3,11,20-trione 21-(21,41-dichlorophenoxy-acetate) is brominated to form the corresponding 2,4-dibromo-compound and is then di-dehydrobrominated to form 1,4-pregnadiene-17 a ,21-diol-3,11,20-trione 21-(21,41-dichlorophenoxyacetate); (5) allopregnane and pregnane-11b ,17 a ,21-triol-3,20-dione 21-(41-chlorophenoxyacetate) are brominated to form the corresponding 2,4-dibromo-compounds and are then dehydrobrominated to form 1,4-pregnadiene-11b ,17 a ,21-triol-3,20-dione 21-(41-chlorophenoxyacetate). Allopregnane - 17 a ,21 - diol - 3,11,20 - trione 21-acetate and allopregnane-11b ,17 a ,21-triol-3,-20-dione 21-acetate are prepared by hydrogenating the corresponding 4-pregnene compounds in the presence of palladium or charcoal. Pregnane - 17 a ,21 - diol - 3,11,20 - trione 21 - (21,41-dichlorophenoxyacetate) is prepared by brominating pregnane-3 a -17 a ,diol-11,20-dione, treating the resulting 21-bromo compound with potassium 2,4-dichlorophenoxyacetate to form pregnane - 3 a ,17 a ,21 - triol - 11,20 - dione 21-(21,41-dichlorophenoxyacetate) and oxidising the last mentioned compound with N-bromosuccinimide. Allopregnane- and pregnane- 11b ,17 a ,21-triol-3,20-dione 21-(41-chlorophenoxyacetate) are prepared by treating allopregnane- and pregnane-11b , 17 a ,21-triol-3,20-dione with 4-chlorophenoxyacetyl chloride in the presence of pyridine. Specifications 735,429, 742,888 and 761,351 also are referred to.
GB5071/57A 1954-11-01 1955-08-03 Process for the production of pregnadienes Expired GB843213A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US843213XA 1954-11-01 1954-11-01

Publications (1)

Publication Number Publication Date
GB843213A true GB843213A (en) 1960-08-04

Family

ID=22184216

Family Applications (1)

Application Number Title Priority Date Filing Date
GB5071/57A Expired GB843213A (en) 1954-11-01 1955-08-03 Process for the production of pregnadienes

Country Status (1)

Country Link
GB (1) GB843213A (en)

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