HRID1605140

反应详情

EQUATION

反应方程式

HRID 1605140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4 g. of citronellol (3,7-dimethyloct-6-en-1-ol), 0.490 g. of p-toluenesulfonic acid and 0.290 g. of hydroquinone is placed in a stainles steel screw cap bomb having an internal volume of 45 ml. The bomb is cooled in dry ice. Methyl mercaptan (9 g.) is introduced directly into the bomb through the valve head. The bomb is sealed, left overnight at room temperature and then heated to 220° in an oil bath for about 72 hours. After cooling in dry ice, the bomb valve is opened and the reaction mixture is carefully poured into 5% aqueous sodium hydroxide solution. Ether is added and the organic layer is separated, washed with 5% NaOH, 5% HCl and water, dired over calcium sulfate and concentrated with vacuo to yield 7-methylthio-3,7-dimethyloctan-1-ol.

WORKUP

后处理

  1. additionA mixture of 4 g
  2. customscrew cap bomb
  3. customThe bomb is sealed
  4. temperatureheated to 220° in an oil bath for about 72 hours
  5. customthe organic layer is separated
  6. washwashed with 5% NaOH, 5% HCl and water
  7. concentrationconcentrated with vacuo