HRID403617

反应详情

EQUATION

反应方程式

HRID 403617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-trifluoromethylpyridine (2.0 g) in ethyl acetate (10 mL) was added bromoacetic acid (1.4 g) at room temperature, and the mixture was heated under reflux overnight. After the reaction mixture was cooled to room temperature, the precipitated solid was collected by filtration, and dried under reduced pressure to give 1-carboxymethyl-4-trifluoromethylpyridinium bromide (1.0 g). To a solution of the obtained compound (1.0 g) in toluene (10 mL) were added acrylonitrile (0.93 g), manganese dioxide (0.91 g) and triethylamine (0.42 g), and the mixture was stirred at 100° C. for 5 hours. The reaction mixture was filtered through a Celite pad, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate) to give the title compound (0.31 g).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux overnight
  3. filtrationthe precipitated solid was collected by filtration
  4. customdried under reduced pressure