HRID1679168

反应详情

EQUATION

反应方程式

HRID 1679168 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

19.4 g (0.1 mole) of N-2,4-xylyl-N'-methyl-thiourea and 15.2 g (0.1 mole) of chloroacetaldehyde-diethylacetal in 150 ml of 2N aqueous hydrochloric acid are refluxed for 1 hour. The clear light-yellow solution is subsequently cooled to room temperature; it is rendered slightly alkaline with 30% aqueous medium hydroxide solution, and extracted with ether. The ether extract is washed with water, dried with sodium sulphate and filtered, and the ether is then distilled off. The oily residue is distilled; b.p. 132°-134° C/0.3 Torr; yield: 20.2 g = 92% of theory.

WORKUP

后处理

  1. extractionextracted with ether
  2. extractionThe ether extract
  3. washis washed with water
  4. dry with materialdried with sodium sulphate
  5. filtrationfiltered
  6. distillationthe ether is then distilled off
  7. distillationThe oily residue is distilled