HRID862564

反应详情

EQUATION

反应方程式

HRID 862564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 6-bromo-2-methoxycarbonylmethyl-N-ethoxalyltetrahydroquinoline (56.0 g, 0.146 mol) in dichloromethane (500 mL) was added dropwise to a suspension of nitronium tetrafluoroborate (25.0 g, 0.179 mol) in dichloromethane (500 mL) at 0° C. The mixture was stirred for 3 h at 0° C., poured into ice-water and extracted with dichloromethane. The organic layer was washed with brine, dried over magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography with 3:1 to 2:1 hexane/ethyl acetate to give 52.0 g of the title compound (83%).

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography with 3:1 to 2:1 hexane/ethyl acetate