HRID385815

反应详情

EQUATION

反应方程式

HRID 385815 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customInto a 50 mL roundbottom flask, was placed
  2. customto react
  3. concentrationThe mixture was concentrated by evaporation under vacuum
  4. customa rotary evaporator
  5. additionThis was followed by the addition of dichloromethane (20 mL)
  6. customto react overnight at room temperature
  7. filtrationThe reaction mixture was filtered
  8. concentrationthe filtrate was concentrated under vacuo
  9. customThe crude mixture was purified by silica gel chromatography (1:40 EtOAc/petroleum ether)