HRID1094716

反应详情

EQUATION

反应方程式

HRID 1094716 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture was refluxed overnight
  2. customquenched with H2O (20 mL)
  3. filtrationThe resultant precipitate was filtered
  4. customdried
  5. customto provide a crude solid which
  6. customwas purified by flash chromatography (Et2O:DCM, 1:1)