تفاعل #42656

معادلة التفاعل

(11β,16β)-21-(acetyloxy)-9-fluoro-11-hydroxy-16-methyl-3,20-dioxopregna-1,4-dien-17-yl propylcarbamate

potassium carbonate

→

title compound

المردود 60.2%

(11β,16β)-9-fluoro-11,21-dihydroxy-16-methyl-3,20-dioxopregna-1,4-dien-17-yl propylcarbamate

المردود 60.2%

المذيبات

tetrahydrofuran

methanol

methanol water

ظروف التفاعل

المعالجة

1. 1
   أخرىthe solution was partitioned between ethyl acetate and water
2. 2
   غسيلthe organic layer was washed with water (twice) and brine
3. 3
   تجفيفdried over Na2SO4
4. 4
   ترشيحThe solution was filtered
5. 5
   أخرىevaporated in vacuo
6. 6
   أخرىto give an oil which
7. 7
   أخرىwas purified by preparative thin layer chromatography on silica gel
8. 8
   غسيلeluting with ethyl acetate/hexane/dichloromethane/methanol (3:3:3:1)

الإجراء التجريبي

To a solution of (11β,16β)-21-(acetyloxy)-9-fluoro-11-hydroxy-16-methyl-3,20-dioxopregna-1,4-dien-17-yl propylcarbamate (8.5 mg, 0.016 mmol) in 0.3 mL of tetrahydrofuran and 0.1 mL of methanol was added 0.030 mL of a 0.1M solution of potassium carbonate in methanol/water (9:1). After 10 minutes at room temperature, the solution was partitioned between ethyl acetate and water and the organic layer was washed with water (twice) and brine and dried over Na2SO4. The solution was filtered and evaporated in vacuo to give an oil which was purified by preparative thin layer chromatography on silica gel, eluting with ethyl acetate/hexane/dichloromethane/methanol (3:3:3:1), to yield 4.6 mg of the title compound as a semi-solid.

المصدر