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
Into a 50 mL roundbottom flask, was placed tert-butyl 4-(trifluoromethylsulfonyloxy)-5,6-dihydropyridine-1(2H)-carboxylate (3.5 g, 10.00 mmol). To this was added dichloromethane (20 mL) followed by the addition of trifluoroacetic acid (5 mL). The resulting solution was allowed to react, with stirring, overnight while the temperature was maintained at room temperature. The mixture was concentrated by evaporation under vacuum using a rotary evaporator. This was followed by the addition of dichloromethane (20 mL). This was followed by the addition of triethylamine (3.03 g, 29.94 mmol). To the mixture was added benzyl chloroformate (2.05 g, 12.02 mmol). The resulting solution was allowed to react overnight at room temperature. The reaction mixture was filtered and the filtrate was concentrated under vacuo. The crude mixture was purified by silica gel chromatography (1:40 EtOAc/petroleum ether) to yield the title compound as a yellow liquid.
WORKUP
后处理
- customInto a 50 mL roundbottom flask, was placed
- customto react
- concentrationThe mixture was concentrated by evaporation under vacuum
- customa rotary evaporator
- additionThis was followed by the addition of dichloromethane (20 mL)
- customto react overnight at room temperature
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated under vacuo
- customThe crude mixture was purified by silica gel chromatography (1:40 EtOAc/petroleum ether)