HRID34142

反应详情

EQUATION

反应方程式

HRID 34142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

10.5 g (50 mmol) dimethyl amino-terephthalate and 8.1 ml (100 mmol) pyridine are dissolved in 175 ml dichloromethane and at −16° C. a solution of 2.7 ml (52.5 mmol) bromine in 25 ml dichloromethane is added dropwise. It is stirred for 4 hours at 0° C. and then heated overnight to ambient temperature. The mixture is added to ice water, washed three times with water and then dried over magnesium sulphate and evaporated down. The crude product is recrystallised from ethanol.

WORKUP

后处理

  1. additionis added dropwise
  2. temperatureheated overnight to ambient temperature
  3. washwashed three times with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated down
  6. customThe crude product is recrystallised from ethanol