HRID597867

反应详情

EQUATION

反应方程式

HRID 597867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 2-chloro-1-(4-chloro-2-fluorophenyl)ethanone (1.5 kg, 5.44 mol), and (E)-N′-(6-chloropyridazin-3-yl)-N,N-dimethylacetimidamide (1.19 kg, 5.72 mol) in DMF (10.14 L) and heat at 120° C. for 5 h. After cooling, add water (30 L) and stir to crystallize the product. Collect the product by filtration and rinse the cake with water (2×12 L) and heptanes (2×10 L) then dry under vacuum to obtain title compound. (1.490 kg, 84.44%; mp=160° C., M+=324).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customto crystallize the product
  3. customCollect the product
  4. filtrationby filtration
  5. washrinse the cake with water (2×12 L) and heptanes (2×10 L)
  6. customthen dry under vacuum