HRID1231

反应详情

EQUATION

反应方程式

HRID 1231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a cold solution (0° C.) of 980 mg (2.8 mmol) of ethyl 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoate (Compound 1) in 5 ml of THF and 10 ml of ethanol was added 78 mg (2 mmol) of sodium borohydride. The mixture was stirred for 6 hours, diluted with water (10 ml) and extracted with Et2O (4×40 ml). The combined organic layers were washed with 10% HCl (5 ml), 10% aqueous NaHCO3 (10 ml) and brine (20 ml), dried over MgSO4 and concentrated in vacuo to give the title compound as a white solid.

WORKUP

后处理

  1. extractionextracted with Et2O (4×40 ml)
  2. washThe combined organic layers were washed with 10% HCl (5 ml), 10% aqueous NaHCO3 (10 ml) and brine (20 ml)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo