HRID1414519

反应详情

EQUATION

反应方程式

HRID 1414519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a chilled (ca 10°) solution of 50.7 g (0.263 mole) of 4-butoxy-2,6-dimethylaniline [Buchi et al., Helv. Chim. Acta, 34, 278 (1951)] in 224 ml glacial acetic acid was added rapidly 62.4 g (.289 mole) of 2-bromo-propionyl bromide and immediately thereafter a chilled (ca 5°) solution of 87.2 g sodium acetate thihydrate in 362 ml water. This mixture was shaken for one-half hour, filtered, washed with water until the washes were neutral, and dried in vacuo over silica gel and KOH; yield 68.9 g (71.6%); m.p. 132.5° - 133.5°. The product was recrystallized from 95% ethanol; m.p. 135.5° - 136°.

WORKUP

后处理

  1. filtrationfiltered
  2. washwashed with water until the washes
  3. dry with materialdried in vacuo over silica gel and KOH
  4. customThe product was recrystallized from 95% ethanol