HRID2224240

反应详情

EQUATION

反应方程式

HRID 2224240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Chloro-5-(4-chlorophenyl)-4-(pyridin-4-yl)pyridazine (5.1 g, 16.9 mmol) was dissolved in pyridine (20 mL) and hydrazine mono-hydrate (17.0 mL, 350.5 mmol) was added. The reaction mixture was stirred at reflux for 40 min. After this time, the reaction mixture was cooled to RT and then concentrated to half of the original volume under reduced pressure. The resultant mixture was diluted with water (100 mL). The yellow colored solid was collected by filtration and rinsed thoroughly with water. The solid was dried in a vacuum oven at 40° C. to give the title compound, 1-(5-(4-chlorophenyl)-4-(pyridin-4-yl)pyridazin-3-yl)hydrazine, (4.4 g, 88%) as a yellow powder. HPLC: 1.01 min; MS, M+H=298.

WORKUP

后处理

  1. temperatureat reflux for 40 min
  2. concentrationconcentrated to half of the original volume under reduced pressure
  3. additionThe resultant mixture was diluted with water (100 mL)
  4. filtrationThe yellow colored solid was collected by filtration
  5. washrinsed thoroughly with water
  6. customThe solid was dried in a vacuum oven at 40° C.