HRID60533

反应详情

EQUATION

反应方程式

HRID 60533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

POCl3 (1 mL) was added to DMF (1 mL) in dioxane (6 mL). 2-Amino-5-{[(1S)-1-phenylethyl]thio}[1,3]thiazolo[4,5-d]pyrimidin-7-ol (1 g, 3.3 mmol) was added to the reaction in one portion. POCl3 (1 mL) was added and the reaction mixture was heated to 80° C. for about 30 min. The reaction was cooled to room temperature and poured onto ice. The resulting mixture was heated at reflux for about 5 h. The mixture was allowed to attain room temperature and was then extracted with EtOAc. The organic layer was passed through a layer of silica gel and concentrated to dryness to give the title compound (1 g, 95% yield).

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. additionpoured onto ice
  3. temperatureThe resulting mixture was heated
  4. temperatureat reflux for about 5 h
  5. customto attain room temperature
  6. extractionwas then extracted with EtOAc
  7. concentrationconcentrated to dryness