HRID1105584

反应详情

EQUATION

反应方程式

HRID 1105584 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

A solution of S-ethyl S-hexyl chlorodithiophosphate (0.03 mole) in methylene chloride (50 ml) is charged into a glass reaction vessel equipped with a mechanical stirrer. Triethylamine (0.03 mole) is added and the mixture is cooled to a temperature of about 0° C. A solution of 3-hydroxylphenylacetaldehyde (0.03 mole) in methylene chloride (15 ml) is slowly added with stirring while maintaining the temperature of the reaction mixture at about 0° C. After the addition is completed, the reaction mixture is allowed to warm to room temperature and stirring is continued for a period of about 1 hour. After this time the reaction mixture is transferred to a separatory funnel and methylene chloride (100 ml) is added. The resulting solution is then washed with water, dilute aqueous sodium hydroxide and again with water. The washed solution is dried over anhydrous magnesium sulfate, is filtered and stripped of solvent under vacuum to yield the desired product S-ethyl S-hexyl O-(3-formylmethylphenyl) dithiophosphate.

WORKUP

后处理

  1. customequipped with a mechanical stirrer
  2. temperaturewhile maintaining the temperature of the reaction mixture at about 0° C
  3. additionAfter the addition
  4. temperatureto warm to room temperature
  5. stirringstirring
  6. customAfter this time the reaction mixture is transferred to a separatory funnel
  7. washThe resulting solution is then washed with water, dilute aqueous sodium hydroxide and again with water
  8. dry with materialThe washed solution is dried over anhydrous magnesium sulfate
  9. filtrationis filtered