HRID1654961

反应详情

EQUATION

反应方程式

HRID 1654961 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

387 mg (1.00 mmol) of ethyl-trans-3-[2-[(4chlorophenyl)sulfonylaminomethyl]indan-5-yl]acrylate was dissolved in 10 ml of ethanol, to which was added 24 mg (0.1 mmol)of nickel chloride·6H2O. Under ice-cooling, to this solution was added 76 mg (2.00 mmol) of sodium borohydride, followed by stirring at room temperature overnight. The ethanol was distilled off, the residue was added with 10 ml of water, and the obtained product was extracted with ethyl acetate, followed by washing and drying then condensing. The obtained crystals were recrystallized from a solvent mixture of hexane and ether to obtain 241 mg colorless crystals. Yield: 62%

WORKUP

后处理

  1. temperatureUnder ice-cooling, to this solution
  2. distillationThe ethanol was distilled off
  3. additionthe residue was added with 10 ml of water
  4. extractionthe obtained product was extracted with ethyl acetate
  5. washby washing
  6. customdrying
  7. customcondensing
  8. customThe obtained crystals were recrystallized from a solvent mixture of hexane and ether