反应详情

Di-tert-butyl azodicarboxylate (1.44 g, 6.26 mmol) was added portionwise at room temperature to a stirred suspension of 4-chloro-7-methoxyquinazolin-6-ol (1.20 g, 5.70 mmol), 2-morpholin-4-ylethanol (0.82 g, 6.26 mmol) and triphenylphosphine (1.8 g, 6.87 mmol) in dichloromethane (25 ml). The reaction mixture was stirred for 2 hour and then the resulting orange solution was purified directly by silica gel chromatography eluting with a mixture of 3% methanol in dichloromethane and then purified further by chromatography on neutral alumina eluting with a 3% mixture of methanol in dichloromethane to give 4-chloro-7-methoxy-6-(2-morpholin-4-ylethoxy)quinazoline (1.40 g, 76% yield) as a pale yellow solid:

1. customthe resulting orange solution was purified directly by silica gel chromatography
2. washeluting with a mixture of 3% methanol in dichloromethane
3. custompurified further by chromatography on neutral alumina eluting with a 3% mixture of methanol in dichloromethane