HRID2421910

反应详情

EQUATION

反应方程式

HRID 2421910 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
68 °C

PROCEDURE

实验过程

2-Amino-6-chloro-3-nitro-benzonitrile (see Goldberg et al., J. Med. Chem., 2003, 1344; 800 mg, 4.05 mmol), 2-methoxyphenylboronic acid (800 mg, 5.26 mmol), and potassium phosphate (2.23 g, 10.5 mmol) were combined in DMA (10 mL) in a flask purged with nitrogen. Tris(dibenzylideneacetone)dipalladium(0) (185 mg, 0.2 mmol) and 2-dicyclohexylphosphino-2′-(N,N-dimethyl-amino)biphenyl (159 mg, 0.4 mmol) were added, and the reaction stirred at 68° C. under nitrogen for 16 h. The solution was diluted with EtOAc (50 mL), and washed with 1N HCl and brine. Organics were dried (MgSO4) and concentrated in vacuo.

WORKUP

后处理

  1. custompurged with nitrogen
  2. washwashed with 1N HCl and brine
  3. dry with materialOrganics were dried (MgSO4)
  4. concentrationconcentrated in vacuo