HRID1094716
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
To a suspension of 5-methyl-6-(4-phenylpiperazine-1-carbonyl)thieno[2,3-d]pyrimidin-4(3H)-one, (0.4 g, 1.13 mmol) in CH3CN (5 mL) was added K2CO3 (0.156 g, mmol), KI (0.182 g, 1.13 mmol), and 2-(4,4-difluoropiperidin-1-yl)acetyl chloride (0.223 g, 1.13 mmol). The reaction mixture was refluxed overnight and then quenched with H2O (20 mL). The resultant precipitate was filtered and dried to provide a crude solid which was purified by flash chromatography (Et2O:DCM, 1:1) providing 0.29 g of pure 3-(2-(4,4-difluoropiperidin-1-yl)-2-oxoethyl)-5-methyl-6-(4-phenyl piperazine-1 carbonyl)thieno[2,3-d]pyrimidin-4(3H)-one, (yield: 50%).
WORKUP
后处理
- temperatureThe reaction mixture was refluxed overnight
- customquenched with H2O (20 mL)
- filtrationThe resultant precipitate was filtered
- customdried
- customto provide a crude solid which
- customwas purified by flash chromatography (Et2O:DCM, 1:1)