HRID1249744
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated to
- temperaturea gentle reflux for 2.5 hours
- customSolvent was removed in vacuo
- customazeotroped with toluene
- dissolutionResidue was dissolved in ethyl acetate
- washwashed with 5% sodium bicarbonate solution
- filtrationfiltered
- customsolvent was removed in vacuo