HRID1259317
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionPost-addition
- stirringthe reaction was stirred at 17-20° C. for 10 hours
- stirringwith stirring
- stirringThe resulting slurry was stirred at 20-25° C. overnight
- filtrationThe title compound was collected by filtration
- washThe cake was washed with water (1 L) and heptane (1 L)
- customdried to constant weight at 40° C.
- customto give 456 g (91%)