HRID1397653

反应详情

EQUATION

反应方程式

HRID 1397653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

35 g (148 mmol) of 4-methylnaphthaleneboronic acid, 33.8 g (124 mmol) of dimethyl 2-bromoisophthalate and 220 ml of 2 M Na2CO3 solution are suspended in 1 l of toluene and 1 l of EtOH, the mixture is saturated with N2, 2.9 g (3 mmol) of tetrakis(triphenylphosphine)palladium(0) are added, and the mixture is heated at the boil for 2 h. The mixture is poured into 3 l of a mixture of water/MeOH/6 M HCl 1:1:1, the beige precipitate is filtered off with suction, washed with water, EtOH and toluene and dried. The content of product according to 1H-NMR is about 95% with an overall yield of 37 g (90%).

WORKUP

后处理

  1. additionare added
  2. temperaturethe mixture is heated at the boil for 2 h
  3. filtrationthe beige precipitate is filtered off with suction
  4. washwashed with water, EtOH and toluene
  5. customdried