HRID1250670
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
268 mg (1.0 mmol) of 2-chloro-7-methyl-4-(3-methyl-2-butenylamino)thieno[3,2-d]pyrimidine and 914 mg (16.0 mmol) of allylamine were heated in a sealed tube at 160° C. for 16 hours. After completion of the reaction, the reaction mixture was allowed to resume room temperature, followed by adding a saturated aqueous sodium hydrogen carbonate solution thereto and extraction with ethyl acetate (50 ml×2). After the organic layer was washed with brine and dried over anhydrous sodium sulfate, the solvent was distilled off. The residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/4) to give 201 mg (yield: 69.8%) of the title compound.
WORKUP
后处理
- customAfter completion of the reaction
- customto resume room temperature
- extractionextraction with ethyl acetate (50 ml×2)
- washAfter the organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was distilled off
- customThe residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/4)