反应详情

To a suspension of 2-(4-chloro-7-methylquinazolin-2-yl)phenol (2.0 g, 7.38 mmol) in CH2Cl2 (25 ml) at 0° C. under an N2 atmosphere was added dropwise a solution of tert-butyl piperidin-4-ylcarbamate (1.92 g, 9.6 mmol) in CH2Cl2 (10 ml) and triethylamine (2.0 ml, 14.76 mmol). The reaction was stirred for 6 hours, then it was quenched with water (25 ml), and the layers were separated. The aqueous phase was extracted twice with CH2Cl2 (10 ml), and the combined organic layers were dried over MgSO4, filtered, and concentrated to give tert-butyl 1-(2-(2-hydroxyphenyl)-7-methylquinazolin-4-yl)piperidin-4-ylcarbamate as a yellow solid (3.24 g, 100%). LC/MS: m/z 435.3 (M+H)+ at 2.79 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).

1. customit was quenched with water (25 ml)
2. customthe layers were separated
3. extractionThe aqueous phase was extracted twice with CH2Cl2 (10 ml)
4. dry with materialthe combined organic layers were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated