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
Trifluoromethanesulfonyl chloride (1.0 ml) was added dropwise to a mixture of 6-hydroxy-3,4-dihydroisoquinolin-1(2H)-one (1.52 g), triethylamine (1.3 ml) and dichloromethane (5 ml), followed by stirring at room temperature for 2 hours. Water was added to the reaction solution, followed by extraction with chloroform, the organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 50:50), and the solvent was evaporated under reduced pressure to obtain, as a colorless powdery solid, 1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl trifluoromethanesulfonate (1.56 g).
WORKUP
后处理
- extractionfollowed by extraction with chloroform
- washthe organic layer was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 50:50)
- customthe solvent was evaporated under reduced pressure