HRID496119

反应详情

EQUATION

反应方程式

HRID 496119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-((2,2-dimethylpropanoyl)amino)phenylboronic acid (2.0 g, 9 mmol), 2-chloropyrimidine (0.8 g, 7 mmol), Pd(PPh3)2Cl2 (100 mg, 2 mol %) 1,2-dimethoxyethane (40 ml) and Na2CO3 (2M, 7 ml, 14 mmol) were refluxed under N2 for 5 h. The mixture was diluted with 10% Na2CO3 (20 ml) and extracted with EtOAc (3×50 ml). The organic layer was dried (Na2SO4) and the solvent was removed in vacuo. The crude product was recrystallised from MeOH/water (1:1) yielding 0.52 g (85%) of N-(4-(2-pyrimidinyl)phenyl)-2,2-dimethylpropanamide as colorless crystals.

WORKUP

后处理

  1. temperaturewere refluxed under N2 for 5 h
  2. extractionextracted with EtOAc (3×50 ml)
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. customthe solvent was removed in vacuo
  5. customThe crude product was recrystallised from MeOH/water (1:1)