HRID1871033

反应详情

EQUATION

反应方程式

HRID 1871033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

40 ml of methanol were added slowly to a mixture of 9.3 g of the ester of Stage C and 4.1 g of sodium borohydride in 100 ml of tetrahydrofuran and the mixture was refluxed for 2 hours. The reaction medium was allowed to return to ambient temperature and was poured into water and neutralized using N hydrochloric acid. Extraction was carried out with dichloromethane and the organic phase was dried. The solvent was evaporated under reduced pressure and the residue was chromatographed on silica (eluant: AcOEt-CH2Cl2 1-1) to obtain 5.8 g of the expected product melting at 100° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. customto return to ambient temperature
  3. extractionExtraction
  4. customthe organic phase was dried
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was chromatographed on silica (eluant: AcOEt-CH2Cl2 1-1)