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
[5-Oxo-1-(3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl)pyrrolidin-3-yl]carbamic acid tert-butyl ester (1.02 g, 2.94 mmol) was added to a solution mixture of trifluoroacetic acid (10 ml) and dichloromethane (10 ml), and the mixture was stirred at room temperature for 3 hours. The reaction solution was concentrated under reduced pressure, the obtained residue was dissolved in water and neutralized by adding a saturated sodium hydrogen carbonate aqueous solution. The solvent of the mixture was removed under reduced pressure and the obtained residue was purified by NH-silica gel column chromatography (chloroform/methanol) to yield 642 mg (88%) of the title compound in the form of a light brown solid.
WORKUP
后处理
- concentrationThe reaction solution was concentrated under reduced pressure
- dissolutionthe obtained residue was dissolved in water
- additionby adding a saturated sodium hydrogen carbonate aqueous solution
- customThe solvent of the mixture was removed under reduced pressure
- customthe obtained residue was purified by NH-silica gel column chromatography (chloroform/methanol)