HRID1250623
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
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
In 2.28 g (40.0 mmol) of allylamine was dissolved 250 mg (0.9 mmol) of 4-benzylamino-2-chloro-7-methylthieno[3,2-d]pyrimidine, and the resulting solution was heated in a sealed tube at 140° C. for 24 hours. After the reaction mixture was cooled, 100 ml of water was added thereto, followed by extraction with ethyl acetate (20 ml×3). The organic layer was washed with 20 ml of water and dried over anhydrous sodium sulfate, and then the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4) to give 217 mg (yield: 81.3%) of the title compound.
WORKUP
后处理
- temperatureAfter the reaction mixture was cooled
- extractionfollowed by extraction with ethyl acetate (20 ml×3)
- washThe organic layer was washed with 20 ml of water
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was distilled off
- customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4)