HRID1036098

反应详情

EQUATION

反应方程式

HRID 1036098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of hydroxylamine hydrochloride (400 mg, 5.8 mmol) in 1 ml water was added to a solution of NaOAc in 1 ml water. To the resulting solution was added 1-acetyl-4-bromo-2-hydroxy-5-methylbenzene (101) (1.14 g, 5 mmol) followed by addition of 15 ml EtOH. The reaction mixture was stirred at 80° C. for 1 h. After concentrated to half of it's volume, the reaction mixture was poured in to 60 ml ice-water. Precipitate formed was filtered, washed with water and dried to give 1.19 g (yield: 97.5%, purity>95%) 5-bromo-2-((hydroxyimino)ethyl)-4-methylphenol (102) as white solid.

WORKUP

后处理

  1. concentrationAfter concentrated to half of it's volume
  2. additionthe reaction mixture was poured in to 60 ml ice-water
  3. customPrecipitate formed
  4. filtrationwas filtered
  5. washwashed with water
  6. customdried