HRID2263088

反应详情

EQUATION

反应方程式

HRID 2263088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-(5-aminopyrimidin-2-yl)acetamide (450 mg, 2.96 mmol) and pyridine (0.718 ml, 8.87 mmol) in tetrahydrofuran (10 ml) was added 2,2,2-trichloroethyl chloroformate (0.612 ml, 4.44 mmol) with ice-cooling, the mixture was stirred for 1 hour with ice-cooling and then at room temperature for 2 hours, the reaction mixture was poured into ice-water and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to obtain the desired product (88.3 mg, 9.1%) as a solid.

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooling
  3. waitat room temperature for 2 hours
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure