HRID968078

反应详情

EQUATION

反应方程式

HRID 968078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 1 l four-necked flask equipped with a thermometer, a stirrer and a dropping funnel, 144.5 g (1.6 mol) of a 50.7% dimethylamine aqueous solution and 118.5 g of water were charged, and 159.4 g (0.38 mol) of a 25% of sulfuric acid aqueous solution was dropwise added over a period of 15 minutes at a temperature of not higher than 20° C. with stirring. Then, 67.4 g (1.38 mol) of sodium cyanide was introduced. Then, 155.1 g (1.25 mol) of 4-fluorobenzaldehyde was dropwise added over a period of 20 minutes at from 20 to 30° C. Thereafter, the reaction was carried out at 50° C. for 4 hours. After completion of the reaction, the reaction mixture was subjected to liquid separation. The organic layer was separated and washed with 500 ml of water of 50° C. to obtain 222.8 g (yield: 98.4%) of the desired compound having a purity of 98.4% (by GC analysis).

WORKUP

后处理

  1. additionwere charged
  2. customAfter completion of the reaction
  3. customthe reaction mixture was subjected to liquid separation
  4. customThe organic layer was separated
  5. washwashed with 500 ml of water of 50° C.