HRID1350912

反应详情

EQUATION

反应方程式

HRID 1350912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

13.3 g (84.0 mmol) of 3-chloro-1,1-dimethyl propylamine-hydrochloride were added to 84.0 mL sodium hydroxide solution (1 M) at 0° C. with vigorous stirring. The reaction mixture was stirred for 30 min at 0° C. and then combined with 50 mL methylene chloride. The phases were separated and the aqueous phase was twice extracted with 35 mL methylene chloride. The combined organic phases were dried over magnesium sulphate and at ambient temperature combined with 14.2 g (81.0 mmol) of 2,6-dichlorobenzaldehyde with stirring. The reaction mixture was stirred for 18 h at ambient temperature, dried again with magnesium sulphate and the solvent was removed. 22.3 g (80.0 mmol, 99%) (3-chloro-1,1-dimethylpropyl)-(2,6-dichlorobenzylidene)-amine were obtained as a yellowish oil.

WORKUP

后处理

  1. customThe phases were separated
  2. extractionthe aqueous phase was twice extracted with 35 mL methylene chloride
  3. dry with materialThe combined organic phases were dried over magnesium sulphate and at ambient temperature
  4. stirringwith stirring
  5. stirringThe reaction mixture was stirred for 18 h at ambient temperature
  6. dry with materialdried again with magnesium sulphate
  7. customthe solvent was removed