HRID1259317

反应详情

EQUATION

反应方程式

HRID 1259317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
18.5 °C

PROCEDURE

实验过程

Methyl 5-methyl-3-oxo-4-[3-(trifluoromethyl)phenyl]-3,4-dihydropyrazine-2-carboxylate (400 g, 1 eq) was dissolved in DMF (3 L) and stirred at 17-20° C. N-Bromosuccinimide (229.3 g, 1 eq) was dissolved in DMF (1 L), and added to the ester solution over 1 hour. Post-addition, the reaction was stirred at 17-20° C. for 10 hours. The reaction mixture was added to water (15 L) with stirring. The resulting slurry was stirred at 20-25° C. overnight. The title compound was collected by filtration. The cake was washed with water (1 L) and heptane (1 L) and then dried to constant weight at 40° C. to give 456 g (91%).

WORKUP

后处理

  1. additionPost-addition
  2. stirringthe reaction was stirred at 17-20° C. for 10 hours
  3. stirringwith stirring
  4. stirringThe resulting slurry was stirred at 20-25° C. overnight
  5. filtrationThe title compound was collected by filtration
  6. washThe cake was washed with water (1 L) and heptane (1 L)
  7. customdried to constant weight at 40° C.
  8. customto give 456 g (91%)