HRID271706

反应详情

EQUATION

反应方程式

HRID 271706 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

23.5 g (150 mmol) 4-chlorophenyl-boric acid are added under argon to a solution of 22.1 g (101 mmol) 5-bromo-3-nitro-pyridin-2-ol, 200 mL (400 mmol) of a 2 M Na2CO3 solution and 731 mg (1.00 mmol) Pd(dppf)Cl2 in 400 mL acetone and 80 mL water. The reaction mixture is stirred for 18 h at 60° C. Acetone is eliminated i.vac. and the residue is adjusted to pH 7 with 160 mL 1 M citric acid. The aqueous phase is extracted three times with EtOAc and once with MeOH. The organic phase is dried over MgSO4 and the solvent is eliminated i.vac. The residue is triturated with EtOAc.

WORKUP

后处理

  1. extractionThe aqueous phase is extracted three times with EtOAc
  2. dry with materialThe organic phase is dried over MgSO4
  3. customThe residue is triturated with EtOAc