HRID1042258
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-(6-bromo-7-methyl-8-nitroquinazolin-4-ylamino)benzonitrile (400 mg, 1.04 mmol) and Pd/C (10%˜30 mg) in EtOH (20 mL) was stirred under H2 gas (1 atm) overnight. 30 mL of NH3/MeOH (2 M) was added and the mixture was filtered through celite and washed with MeOH/DCM (˜1:1). After removal of solvent the product was purified by flash chromatography eluting with MeOH/DCM (1-5%) to give 4-(8-amino-7-methylquinazolin-4-ylamino)benzonitrile (238 mg, 83%). MS (ESI, pos. ion) m/z: 276 [M+H]+
WORKUP
后处理
- filtrationthe mixture was filtered through celite
- washwashed with MeOH/DCM (˜1:1)
- customAfter removal of solvent the product
- customwas purified by flash chromatography
- washeluting with MeOH/DCM (1-5%)