GB909373A - Improvements in or relating to steroids - Google Patents

Improvements in or relating to steroids

Info

Publication number
GB909373A
GB909373A GB4001360A GB4001360A GB909373A GB 909373 A GB909373 A GB 909373A GB 4001360 A GB4001360 A GB 4001360A GB 4001360 A GB4001360 A GB 4001360A GB 909373 A GB909373 A GB 909373A
Authority
GB
United Kingdom
Prior art keywords
alkyl
methoxy
pyranyl
oxy
alkenyl
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
GB4001360A
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.)
GD Searle LLC
Original Assignee
GD Searle LLC
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 GD Searle LLC filed Critical GD Searle LLC
Publication of GB909373A publication Critical patent/GB909373A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J1/00Normal steroids containing carbon, hydrogen, halogen or oxygen, not substituted in position 17 beta by a carbon atom, e.g. estrane, androstane
    • 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

The invention comprises 16a -(alkyl, alkenyl, and alkynyl)-17b -ol and 16b -(alkyl, alkenyl and alkynyl)-17a -ol steroid compounds of the general formula <FORM:0909373/IV (b)/1> in which there is one double bond in the 4(5) or 5(10) position and wherein R represents hydrogen or an alkyl radical having less than 9 carbon atoms or an alkylacyl radical in which the alkyl portion contains less than 8 carbon atoms, R1 represents an alkyl, alkenyl or alkynyl radical having less than 9 carbon atoms, and R11 represents hydrogen or an alkylacyl radical in which the alkyl portion contains less than 8 carbon atoms; a process for the preparation of steroid compounds of the general formula <FORM:0909373/IV (b)/2> wherein R and R1 have the above significance, by isomerising 5(10)-estrene compounds of the general formula <FORM:0909373/IV (b)/3> wherein R and R1 have the above significance, with an acid (this process may be modified by treating a 3-alkoxy-16-alkyl, alkenyl or alkynyl-2,5(10)-estradiene-16,17-diol or the corresponding 17-ether with mild acid to form a 5(10)-estrene of the above general formula which may or may not be isolated before forming the 4-estrene by continuing the acid treatment-a 17b -(2-pyranyl)oxy ether may also be used in which case the 4-estrene product contains a 17b -hydroxy group), and when R represents the alkylacyl radical, acylating the product with the required acid anhydride; a process for the preparation of compounds of the general formula <FORM:0909373/IV (b)/4> wherein R1 represents an alkyl or alkenyl radical containing less than 9 carbon atoms, by hydrogenating compounds of the general formula <FORM:0909373/IV (b)/5> wherein R11 represents an alkenyl or alkynyl radical containing less than 9 carbon atoms; a process for the preparation of compounds of the general formula <FORM:0909373/IV (b)/6> wherein R represents hydrogen, an alkyl radical containing less than 9 carbon atoms or an alkylacyl radical in which the alkyl portion contains less than 8 carbon atoms, R1 represents an alkyl, alkenyl or alkynyl radical containing less than 9 carbon atoms, and R11 represents hydrogen or an alkylacyl radical in which the alkyl portion contains less than 8 carbon atoms, by hydrolysing compounds of the general formula <FORM:0909373/IV (b)/7> wherein A represents an alkyl or acyl radical, and R, R1 and R11 have the significance indicated immediately above. The 16- and/or 17-esterified 5(10)-estrenes of the above general formula are prepared by acylating with one equivalent of an acylating agent to form the 17-monoester or with two equivalents to form the 16,17-diester, or by selectively hydrolysing the 16,17-diester to form the 16-monoester. The 16-substituted-16,17-dihydroxy-4-estrene-3-ones of the above general formula may be 17-monoacylated, or diacylated, e.g. with isopropenyl acetate followed by hydrolysis of the group in the 3-position of the resulting 16-substituted-3,16b ,17b -triacetoxy-3,5-estradiene. 3-Alkoxy-16-alkyl, alkenyl or alkynyl-2,5(10)-estradiene-16,17-diol or the corresponding 17-ether is prepared by a Birch type reduction, i.e. with lithium and ammonia, of the corresponding 3-alkoxy-16-alkyl, alkenyl, or alkynyl-1,3,5(10) - estradiene - 16,17 - diol or 17-ether thereof. 3,17b -Dimethoxy-16a -propyl-1,3,5(10) - estratrien-16b -ol is prepared by reacting 3-methoxy - 16a - propyl - 1,3,5(10) - estratriene-16b ,17b -diol with potassium t-butoxide and then with methyl iodide. 3-Methoxy-16a -propyl-17b -ethoxy-1,3,5(10)-estratrien-16b -ol is prepared by a similar method. 3 - Methoxy-16a -ethynyl-17b -(2-pyranyl)oxy-2,5(10) -estradien-16b -ol is prepared by reducing 3-methoxy - 17b - (2-pyranyl)oxy-1,3,5(10)-estratrien-16-one with sodium borohydride to form 3-methoxy-17b -(2-pyranyl)oxy-1,3,5(10)-estratrien-16b -ol, reducing this compound with sodium and ammonia to form 3-methoxy-17b -(2-pyranyl)oxy-2,5(10)-estradien-16b -ol, oxidising this compound by the Oppenauer method to form 3-methoxy-17b -(2-pyranyl)oxy-2,5(10)-estradien-16-one, and reacting this compound with potassium acetylide to form the desired product. 3-Methoxy - 16a - (1-octynyl)-17b -(2-pyranyl)-oxy-2,5(10)-estradien-16b -ol is prepared by reacting 1-octyne magnesium bromide and 3-methoxy-17b -(2-pyranyl)oxy-2,5(10) - estradien16 - one. 3 - Methoxy-16a -(2-methallyl)-17b -(2-pyranyl)oxy-2,5(10) -estradien-16a -ol and 3-methoxy-16a -allyl-17b -(2-pyranyl)oxy - 2.5(10)-estradien-16b -ol are prepared by a similar method. 3-Alkoxy-16a -alkyl, alkenyl or alkynyl-estra-3,5-diene-16b ,17b -diol is prepared by treating 3-methoxy - 17b - (2-pyranyl)oxy-2,5(10)-estradien-16-one with hydrochloric acid to form 17b -hydroxy-4-estrene-3,16-dione, treating this compound with an alkyl orthoformate to form 3-alkoxy-17a -hydroxy-3,5-estradien-16-one, and treating this compound with an alkyl, alkenyl or alkynyl metallic reagent such as an alkyl magnesium halide or an alkyl lithium. 3-Methoxy - 16a - octyl-17b -(2-pyranyl)oxy-2,5(10)-estradiene-17b -ol 16-monoacetic ester is prepared by passing ketene gas into a solution of 3 - methoxy - 16a - octyl-17b -(2-pyranyl)oxy-2,5(10)-estradien-16b -ol. 3 - Methoxy - 16a - octyl-2,5(10)-estradiene-16b ,17b -diol 17-monoacetic ester and 16,17-diacetic ester are prepared by reacting 3-methoxy-16a -octyl-2,5(10)-estradiene - 16b ,17b -diol with one and two equivalents respectively of acetic anhydride. The 16,17-diacetic ester may be selectively hydrolysed to form the 16-monoacetic ester. The process is applicable to the preparation of the 3-alkoxy-16a -substituted-2,5(10)-estradiene-16b ,17b -diol, 16- and 17-monoacylates and 16,17-diacylates.
GB4001360A 1959-11-23 1960-11-21 Improvements in or relating to steroids Expired GB909373A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US85460659A 1959-11-23 1959-11-23

Publications (1)

Publication Number Publication Date
GB909373A true GB909373A (en) 1962-10-31

Family

ID=25319143

Family Applications (1)

Application Number Title Priority Date Filing Date
GB4001360A Expired GB909373A (en) 1959-11-23 1960-11-21 Improvements in or relating to steroids

Country Status (2)

Country Link
BE (1) BE597322A (en)
GB (1) GB909373A (en)

Also Published As

Publication number Publication date
BE597322A (en) 1961-05-23

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