HRID1094726

反应详情

EQUATION

反应方程式

HRID 1094726 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 6-(4-(3-chlorophenyl)piperazine-1-carbonyl)-5-methylthieno[2,3-d]pyrimidin-4(3H)-one, (0.1 g, 0.26 mmol) in CH3CN (5 mL) was added K2CO3 (36 mg, 0.26 mmol), KI (43 mg, 0.26 mmol), and 2-chloro-N-ethyl-N-(2,2,2-trifluoroethyl)acetamide, (52 mg, 0.26 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 30 mg of pure 2-(6-(4-(3-chlorophenyl)piperazine-1-carbonyl)-5-methyl-4-oxothieno[2,3-d]pyrimidin-3 (4H)-yl)-N-ethyl-N-(2,2,2-trifluoroethyl)acetamide, (yield: 21%).

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)