HRID1759517

反应详情

EQUATION

反应方程式

HRID 1759517 的结构方程式

PROCEDURE

实验过程

A mixture of 3-chlorocinnamic acid (25 g.), thionyl chloride (19.4 g.) and benzene (300 ml.) was heated under reflux for 2 hours, then evaporated under reduced pressure on a rotary evaporator to give an oil. The oil was dissolved in benzene (50 ml.), and the benzene solution was added slowly to a mixture of isopropylamine (25 g.) and benzene (300 ml.). The resulting mixture was allowed to stir at room temperature for 2 hours, and heated under mild reflux for 1 hour. It was then allowed to set at room temperature overnight. The precipitate thus separated was collected on a filter, and washed with benzene. The combined filtrate and washings were washed with water, then dried over potassium carbonate. Removal of benzene under reduced pressure on a rotary evaporator gave an oil which solidified on standing. The product melted at 92°-94°, and weighed 28 g.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. customevaporated under reduced pressure on a rotary evaporator
  4. customto give an oil
  5. temperatureheated
  6. temperatureunder mild reflux for 1 hour
  7. waitto set at room temperature overnight
  8. customThe precipitate thus separated
  9. customwas collected on a filter
  10. washwashed with benzene
  11. washThe combined filtrate and washings were washed with water
  12. dry with materialdried over potassium carbonate
  13. customRemoval of benzene under reduced pressure
  14. customon a rotary evaporator
  15. customgave an oil which