HRID1249744

反应详情

EQUATION

反应方程式

HRID 1249744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7H-[1,3]dioxolo[4,5-g]quinazolin-8-one (0.550 g, 2.78 mmol) and phosphorus pentachloride (0.800 g, 3.84 mmol) in 3 mL phosphorus oxychloride was heated to a gentle reflux for 2.5 hours. Solvent was removed in vacuo, and azeotroped with toluene. Residue was dissolved in ethyl acetate and washed with 5% sodium bicarbonate solution and then filtered, and then solvent was removed in vacuo to give 8-chloro-[1,3]dioxolo[4,5-g]quinazoline (0.400 g, 74%).

WORKUP

后处理

  1. temperaturewas heated to
  2. temperaturea gentle reflux for 2.5 hours
  3. customSolvent was removed in vacuo
  4. customazeotroped with toluene
  5. dissolutionResidue was dissolved in ethyl acetate
  6. washwashed with 5% sodium bicarbonate solution
  7. filtrationfiltered
  8. customsolvent was removed in vacuo