反应详情

To a solution of (±)-{2-[1-(3-benzyl-7-chloro-4-oxo-3,4-dihydro-quinazolin-2-yl)-2-methyl-propylamino]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester (1.62 g, 3.16 mmol) in dichloromethane (40 mL) was added trifluoroacetic acid (10 mL). The resultant solution was maintained at ambient temperature overnight and concentrated under reduced pressure. The residue was dissolved in dichloromethane (50 mL) and washed with saturated aqueous sodium bicarbonate (40 mL). The aqueous layer was extracted with dichloromethane (50 mL) and the combined extracts were dried over magnesium sulfate, filtered and concentrated under reduced pressure to give (±)-2-[1-(2-amino-2-methyl-propylamino)-2-methyl-propyl]-3-benzyl-7-chloro-3H-quinazolin-4-one (1.29 g, 99%) as a yellow solid which was used in the subsequent step without purification.

1. concentrationconcentrated under reduced pressure
2. dissolutionThe residue was dissolved in dichloromethane (50 mL)
3. washwashed with saturated aqueous sodium bicarbonate (40 mL)
4. extractionThe aqueous layer was extracted with dichloromethane (50 mL)
5. dry with materialthe combined extracts were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure