HRID1250607
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 150 mg (0.57 mmol) of 4-allylamino-2-chloro-6-nitroquinazoline, 772 mg (5.70 mmol) of 2,2,2-trifluoroethylamine and 1.15 g (11.4 mmol) of triethylamine was stirred in a sealed tube at room temperature for 16 hours. After completion of the reaction, ice water was added to the reaction mixture, followed by extraction with chloroform (10 ml×3). After the organic layer was washed with brine and then dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by a silica gel chromatography to give 57 mg (yield: 30.8%) of the title compound.
WORKUP
后处理
- additionwas added to the reaction mixture
- extractionfollowed by extraction with chloroform (10 ml×3)
- washAfter the organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by a silica gel chromatography