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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
6-[(4R)-4-{[3-(7-Methoxy-2-oxoquinoxalin-1(2H)-yl)propyl]amino}-2-oxopyrrolidin-1-yl]-2H-1,4-benzoxazin-3(4H)-one (2.86 g, 6.17 mmol) was dissolved in dichloromethane (50 ml) and ethanol (2 ml). To this solution was added 4 N hydrogen chloride/dioxane solution (1.59 ml, 6.37 mmol) under cooling in an ice bath. The precipitated insoluble material was collected by filtration and was then dried. The obtained residue was suspended in ethanol (20 ml), and the suspension was then stirred at 50° C. for 20 minutes. The suspension was cooled in an ice bath, and the insoluble material was collected by filtration. The filtrate was dried at 70° C. overnight under reduced pressure to yield 2.36 g (74%) of the above-captioned compound in the form of a colorless solid.
WORKUP
后处理
- temperatureunder cooling in an ice bath
- filtrationThe precipitated insoluble material was collected by filtration
- customwas then dried
- temperatureThe suspension was cooled in an ice bath
- filtrationthe insoluble material was collected by filtration
- customThe filtrate was dried at 70° C. overnight under reduced pressure