HRID868148
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
To a suspension of 1,4-dihydro-6,7-dimethoxy-4-oxo-N-(2-oxo-1-imidazolidinyl)-3-quinolinecarboxamide (23.1 g, 69.5 mmol) in 1.2 l of dichloromethane, a solution of boron tribromide (104.5 g, 417 mmol) was added dropwise at 0° C. After stirring for 3 days at room temperature, the precipitate was filtered off, washed with dichloromethane and was then added to 300 ml of methanol under ice cooling. After stirring for 2 hours, the solid was filtered off, washed with methanol and dried in vacuo. Yield: 24.8 g (still contained some starting material). The reaction was repeated to give 18.4 g of the title compound after methanol treatment, melting point>300° C.
WORKUP
后处理
- filtrationthe precipitate was filtered off
- washwashed with dichloromethane
- additionwas then added to 300 ml of methanol under ice cooling
- stirringAfter stirring for 2 hours
- filtrationthe solid was filtered off
- washwashed with methanol
- customdried in vacuo