HRID2180593

反应详情

EQUATION

反应方程式

HRID 2180593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-(4-bromo-3-methoxy-5,5-dimethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-ethanone (Compound A-93, 12.1 g, 39 mmol) in ethanol (250 mL) was added sodium borohydride (741 mg, 19.5 mmol). After heating to reflux for 2 h the mixture was cooled to room temperature, quenched with 10% HCl and extracted with diethyl ether. The combined ethereal layers were washed with water, brine, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as a colorless syrup. The material was used in the next step without further purification.

WORKUP

后处理

  1. temperatureAfter heating
  2. temperatureto reflux for 2 h the mixture
  3. customquenched with 10% HCl
  4. extractionextracted with diethyl ether
  5. washThe combined ethereal layers were washed with water, brine
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo