HRID1354322
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 suspension of 2-(5-chloro-2-fluorophenyl)-5,6,7,8-tetrahydroquinazolin-4-ol (500 mg, 1.89 mmol) in POCl3 (6 ml) was stirred under reflux for 1 h. The solution was then cooled to room temperature and concentrated under reduced pressure to afford a white solid which was dissolved in methylene chloride. The solution was cooled to 0° C. and ice was added followed by sat. NaHCO3. The organic layer was separated, washed with brine, dried (MgSO4), filtered and evaporated in vacuo to provide a crude white solid 4-Chloro-2-(5-chloro-2-fluorophenyl)-5,6,7,8-tetrahydroquinazoline which was not further purified.
WORKUP
后处理
- temperatureunder reflux for 1 h
- concentrationconcentrated under reduced pressure
- customto afford a white solid which
- temperatureThe solution was cooled to 0° C.
- additionice was added
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated in vacuo