HRID590996

反应详情

EQUATION

反应方程式

HRID 590996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 2-(tert-butoxy)-2-[2-(3,4-dihydro-2H-1-benzopyran-6-yl)-5-phenylthiophen-3-yl]acetate (11j) (57 mg, 0.13 mmol) and potassium hydroxide (64 mg, 0.52 mmol) in a mixture of ethanol (2 mL) and water (6 mL) was refluxed for 4 hours. The mixture was concentrated in vacuo. Water (5 mL) was added and the aqueous layer was washed with diethyl ether (5 mL), then extracted with dichloromethane (5 mL). The organic layer was washed with 1N hydrochloric acid (5 mL), dried over sodium sulfate and evaporated to dryness to provide the desired acid (45 mg, 0.11 mmol, 81%) as a white solid.

WORKUP

后处理

  1. temperaturewas refluxed for 4 hours
  2. concentrationThe mixture was concentrated in vacuo
  3. additionWater (5 mL) was added
  4. washthe aqueous layer was washed with diethyl ether (5 mL)
  5. extractionextracted with dichloromethane (5 mL)
  6. washThe organic layer was washed with 1N hydrochloric acid (5 mL)
  7. dry with materialdried over sodium sulfate
  8. customevaporated to dryness