HRID1250595
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
After 100 mg (0.41 mmol) of 4-allylamino-2-amino-6-nitroquinazoline was dissolved in 10 ml of acetonitrile, 84 mg (0.82 mmol) of acetic anhydride and 0.06 ml (0.45 mmol) of triethylamine were added thereto, and then the reaction mixture was subjected to heating under reflux overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate, washing successively with a saturated aqueous sodium hydrogen carbonate solution and brine and drying over anhydrous sodium sulfate. The solvent was distilled off, followed by recrystallization from ethyl acetate-hexane to give 95 mg (80.7%) of the title compound.
WORKUP
后处理
- temperatureto heating
- temperatureunder reflux overnight
- extractionfollowed by extraction with ethyl acetate
- washwashing successively with a saturated aqueous sodium hydrogen carbonate solution and brine
- dry with materialdrying over anhydrous sodium sulfate
- distillationThe solvent was distilled off
- customfollowed by recrystallization from ethyl acetate-hexane