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
Ethyl acetate (2.0 mL) was added to dimethylcarbamic acid 4-fluoromethyl-3-(2-fluoro-3-nitrobenzyl)-2-oxo-2H-1-benzopyran-7-yl ester (20.5 mg) (6c-1-4), and tin(II) chloride dihydrate (60 mg) was added to the resultant suspension while stirring at room temperature. The suspension was heated under reflux for 1.5 hours, and after cooling to room temperature, saturated sodium hydrogen carbonate was added, and the mixture was extracted with ethyl acetate. The resultant organic layer extraction liquid was washed with saturated saline, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was then distilled away under reduced pressure to yield the title compound (19.5 mg).
WORKUP
后处理
- temperatureThe suspension was heated
- temperatureunder reflux for 1.5 hours
- temperatureafter cooling to room temperature
- extractionthe mixture was extracted with ethyl acetate
- extractionThe resultant organic layer extraction liquid
- washwas washed with saturated saline
- dry with materialthe organic layer was dried over anhydrous magnesium sulfate
- distillationThe solvent was then distilled away under reduced pressure