HRID1637167
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
1.9 g hexahydro-7-phenyl-1,4-diazepin-5-one (for preparation see Example 1C) in 30 ml acetonitrile were heated to boiling with 2.0 g potassium carbonate and 1.2 g benzyl chloride with reflux cooling for 36 hours. Then filtration was carried out and the filtrate reduced in volume. The remaining residue was shaken with 10% aqueous citric acid solution, the organic phase was separated, dried over magnesium sulfate and reduced in volume under a vacuum. 2.23 g crude 1-benzyl-hexahydro-7-phenyl-1,4-diazepin-5-one were obtained as an oil, which was used for the next synthesis stage without further purification or characterization.
WORKUP
后处理
- temperaturewith reflux
- temperaturecooling for 36 hours
- filtrationThen filtration
- customthe organic phase was separated
- dry with materialdried over magnesium sulfate