HRID450588

反应详情

EQUATION

反应方程式

HRID 450588 的结构方程式

PROCEDURE

实验过程

To N-(3-(dimethylamino)propyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-sulfonamide (0.6 g, 1.8 mmol) was added phosphorus oxychloride (5.0 mL, 36 mmol) and the suspension heated at reflux for 1.5 hours. The reaction was cooled to ambient temperature and the excess phosphorus oxychloride removed under vacuum. The residue was co-evaporated several times with chloroform. Drying under vacuum gave a hydroscopic cream solid that was used without further purification (0.65 g, 92%).

WORKUP

后处理

  1. temperaturethe suspension heated
  2. temperatureat reflux for 1.5 hours
  3. customthe excess phosphorus oxychloride removed under vacuum
  4. customDrying under vacuum
  5. customgave a hydroscopic cream solid that
  6. customwas used without further purification (0.65 g, 92%)