HRID2118504

反应详情

EQUATION

反应方程式

HRID 2118504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

The N-formyl-2(3,4-dimethoxy-phenyl)-ethylamine so obtained is stirred with polyphosphoric acid (1 kg) and heated to 140° C. (oil bath temperature). The reaction mixture foams vigorously starting from an internal temperature of 70° C. After 30 minutes, an internal temperature of about 140° C. is attained. The mixture is then poured onto water (1 liter) and made alkaline with concentrated ammonia (1.8 liters) while ice is added. The reaction product is extracted repeatedly with ethyl acetate, the ethyl acetate phase is washed with water, dried, over magnesium sulphate and evaporated giving the title compound (142.5 g) as an oil.

WORKUP

后处理

  1. customvigorously starting from an internal temperature of 70° C
  2. customan internal temperature of about 140° C.
  3. additionThe mixture is then poured onto water (1 liter)
  4. additionis added
  5. extractionThe reaction product is extracted repeatedly with ethyl acetate
  6. washthe ethyl acetate phase is washed with water
  7. dry with materialdried, over magnesium sulphate
  8. customevaporated