HRID1732239

反应详情

EQUATION

反应方程式

HRID 1732239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

In a two liter bottle were mixed 4-butoxy-2,6-dimethylaniline (50.7 g, 0.263 mole) and glacial acetic acid (224 ml) and the mixture was cooled to about 10° C. To this was added and mixed rapidly 2-bromopropionyl bromide (62.4 g, 0.289 mole) immediately followed by a precooled (5° C.) solution of sodium acetate trihydrate (87.2 g) in water (362 ml). The whole was vigorously shaken to ensure intimate mixture of the components. After 30 min. of mechanical shaking, the precipitate was filtered off and washed carefully with distilled water. It was thereafter dried. The yield was 68.9 g (72%). Recrystallized from 95% ethanol, it melted at 135.5°-136°.

WORKUP

后处理

  1. additionTo this was added
  2. additionmixture of the components
  3. filtrationthe precipitate was filtered off
  4. washwashed carefully with distilled water
  5. customIt was thereafter dried
  6. customRecrystallized from 95% ethanol, it melted at 135.5°-136°