HRID704140

反应详情

EQUATION

反应方程式

HRID 704140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diethyl 2-benzylthiomethyl-2-isobutylmalonate (32.0 g.) in dry diethyl ether (60 ml.) was added to a stirred suspension of lithium aluminium hydride (7.0 g.) in dry diethyl ether (400 ml.), at 0°, under nitrogen. The mixture was stirred at room temperature for three hours and then refluxed with stirring for a further three hours. The mixture was cooled and 10% aqueous sodium hydroxide solution (25 ml.) was added very carefully. The mixture was filtered and the solid was washed with ether. The filtrates were dried over anhydrous magnesium sulphate and evaporated in vacuo. 2-Benzylthiomethyl-2-isobutyl-propan-1,3-diol was obtained as a colourless solid (20 g.) and was used without further purification.

WORKUP

后处理

  1. temperaturerefluxed
  2. stirringwith stirring for a further three hours
  3. temperatureThe mixture was cooled
  4. filtrationThe mixture was filtered
  5. washthe solid was washed with ether
  6. dry with materialThe filtrates were dried over anhydrous magnesium sulphate
  7. customevaporated in vacuo