反应详情

To a solution (76 ml) of 6-chloro-2-methylamino-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid (3.8 g) in THF were added triethylamine (4.0 ml) and benzyl chloroformate (3.6 ml) at 0° C. with stirring, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate and the mixture was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=2/1-dichloromethane/methanol/acetic acid=50/10/1) to give the title compound (2.5 g) as yellow powder.

1. stirringthe mixture was stirred at room temperature for 1 hr
2. extractionthe mixture was extracted with ethyl acetate
3. dry with materialThe organic layer was dried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=2/1-dichloromethane/methanol/acetic acid=50/10/1)