HRID53453

反应详情

EQUATION

反应方程式

HRID 53453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl-17β-[3-(4-carboxyphenyl)propionyl]-estra-1,3,5(10)-triene-3-carboxylate (0.053 g, 0.11 mmoles), K2CO3 (50 mg, 0.36 mmoles), MeOH (9 ml) and H2O (1 ml) was refluxed under argon. Methanol was evaporated and the residue was acidified with dilute HCl. Extracted with EtOAc. The organic layer was washed with H2O, brine, dried and concentrated. The residue was chromatographed (silica gel) eluting with 1% MeOH in CH2Cl2 containing 1% HOAC to give the title compound as a white solid (40 mg, 80%), mp 285°-290° C.

WORKUP

后处理

  1. temperaturewas refluxed under argon
  2. customMethanol was evaporated
  3. extractionExtracted with EtOAc
  4. washThe organic layer was washed with H2O, brine
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was chromatographed (silica gel)
  8. washeluting with 1% MeOH in CH2Cl2 containing 1% HOAC