HRID1494671

反应详情

EQUATION

反应方程式

HRID 1494671 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,2-Di(benzylthiomethyl)pentan-1-ol (8.0 g.) in dry diethyl ether (150 ml) was added to liquid ammonia (500 ml) which was stirred under nitrogen at -70° . Sodium (8.0 g.) was added in small pieces and the mixture was stirred at -70° for 3 hours. The mixture was allowed to warm to 20° and solid ammonium chloride (20 g.) was added. This was followed by careful addition of methanol (100 ml) to destroy excess sodium. Water (200 ml) was added and the aqueous mixture was extracted with diethyl ether. The ethereal extracts were dried over anhydrous magnesium sulphate and evaporated in vacuo. 2-Hydroxymethyl-2-n-propylpropan-1,3-dithiol was obtained as a colourless oil (4.6 g.).

WORKUP

后处理

  1. stirringthe mixture was stirred at -70° for 3 hours
  2. temperatureto warm to 20°
  3. customto destroy excess sodium
  4. additionWater (200 ml) was added
  5. extractionthe aqueous mixture was extracted with diethyl ether
  6. dry with materialThe ethereal extracts were dried over anhydrous magnesium sulphate
  7. customevaporated in vacuo