HRID496119
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewere refluxed under N2 for 5 h
- extractionextracted with EtOAc (3×50 ml)
- dry with materialThe organic layer was dried (Na2SO4)
- customthe solvent was removed in vacuo
- customThe crude product was recrystallised from MeOH/water (1:1)