HRID1257457

反应详情

EQUATION

反应方程式

HRID 1257457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the compound (300 mg, 0.759 mmol) obtained in Example 186b were added ethanol (4 mL), tetrahydrofuran (2 mL) and 2N aqueous sodium hydroxide solution (0.76 mL, 1.52 mmol), and the mixture was stirred overnight. The reaction mixture was extracted with water, and washed with ether. The aqueous layer was acidified with 6N hydrochloric acid, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate), and recrystallized from ethanol-hexane to give the title compound (186 mg, 64%) as colorless crystals.

WORKUP

后处理

  1. extractionThe reaction mixture was extracted with water
  2. washwashed with ether
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)
  8. customrecrystallized from ethanol-hexane