HRID972871

反应详情

EQUATION

反应方程式

HRID 972871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a well stirred solution of 0.11 mole of thiourea in 250 ml. methanol, under N2 is added 0.1 mole of 3-benzyloxy-4-chloromethyl-2-methyl-5-vinylpyridine hydrochloride. The mixture is refluxed for 1 hour and then cooled. A solution of 0.4 mole of sodium hydroxide in 50 ml. of water is added, and the resulting mixture refluxed for 30 minutes. After concentration in vacuo the reaction mixture is taken up between benzene and water and enough acetic acid added to neutralize the mixture. The organic layer is separated, washed well with water, dried, and concentrated to give 2-methyl-3-benzyloxy-4-mercaptomethyl-5-vinylpyridine.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 1 hour
  2. temperaturecooled
  3. temperaturethe resulting mixture refluxed for 30 minutes
  4. concentrationAfter concentration in vacuo the reaction mixture
  5. additionadded
  6. customThe organic layer is separated
  7. washwashed well with water
  8. customdried
  9. concentrationconcentrated