HRID14378

反应详情

EQUATION

反应方程式

HRID 14378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customthe solution was partitioned between ethyl acetate and water
  2. washthe organic layer was washed with water (twice) and brine
  3. dry with materialdried over Na2SO4
  4. filtrationThe solution was filtered
  5. customevaporated in vacuo
  6. customto give an oil which
  7. customwas purified by preparative thin layer chromatography on silica gel
  8. washeluting with ethyl acetate/hexane/dichloromethane/methanol (3:3:3:1)