HRID874347

反应详情

EQUATION

反应方程式

HRID 874347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

2-Bromo-1-(2,5-difluorophenyl)ethanone (1.5 g) was added to an ethanol (8.2 ml) solution of methyl 2-aminoisonicotinate (1.0 g), and the obtained mixture was then stirred in a nitrogen atmosphere at 60° C. for 18 hours. Thereafter, 2-bromo-1-(2,5-difluorophenyl)ethanone (0.77 g) was added to the reaction solution, and the obtained mixture was then stirred for 6 hours at the same temperature as described above. Thereafter, the reaction solution was concentrated under reduced pressure, and ethyl acetate (10 ml) was then added to the obtained residue. The precipitated solid was collected by filtration, and it was washed with ethyl acetate (15 ml) and heptane (6 ml) and was then dried, so as to obtain the title compound (2.5 g) in the form of a pink solid.

WORKUP

后处理

  1. stirringthe obtained mixture was then stirred for 6 hours at the same temperature
  2. concentrationThereafter, the reaction solution was concentrated under reduced pressure, and ethyl acetate (10 ml)
  3. additionwas then added to the obtained residue
  4. filtrationThe precipitated solid was collected by filtration, and it
  5. washwas washed with ethyl acetate (15 ml) and heptane (6 ml)
  6. customwas then dried