反应详情

温度

0 °C

Potassium carbonate (1.60 g, 12.6 mmol) was added to a solution of tert-butyl (2R)-2-{[(3-{[(2,2-dimethylpropanoyl)oxy]methyl}-7-hydroxy-4-oxo-3,4-dihydroquinazolin-5-yl)oxy]methyl}pyrrolidine-1-carboxylate (1.50 g, 3.2 mmol) in dimethylformamide (10 ml) and the mixture stirred at 0° C. for 5 minutes. Dimethyl sulphate (0.6 ml, 6.3 mmol) was added and the reaction stirred at 0° C. for a further 5 minutes and then warmed to room temperature and stirred for 1 hour. The reaction mixture was evaporated under reduced pressure and the residue dissolved in dichloromethane (20 ml) and washed with water (2×20 ml). The organics were dried over magnesium sulphate, filtered and evaporated under reduced pressure to give tert-butyl (2R)-2-{[(3-{[(2,2-dimethylpropanoyl)oxy]methyl}-7-methoxy-4-oxo-3,4-dihydroquinazolin-5-yl)oxy]methyl}pyrrolidine-1-carboxylate (0.750 g, 48% yield) which was used in the next stage without further purification.

1. stirringthe reaction stirred at 0° C. for a further 5 minutes
2. temperaturewarmed to room temperature
3. stirringstirred for 1 hour
4. customThe reaction mixture was evaporated under reduced pressure
5. dissolutionthe residue dissolved in dichloromethane (20 ml)
6. washwashed with water (2×20 ml)
7. dry with materialThe organics were dried over magnesium sulphate
8. filtrationfiltered
9. customevaporated under reduced pressure