HRID1930063

反应详情

EQUATION

反应方程式

HRID 1930063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2-Bromo-1-(2,4-difluorophenyl)-2-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone (0.500 g, 1.26 mmol, Preparation #A.2) and urea (0.228 g, 3.80 mmol) were added to DMF (5 mL) then heated at about 100° C. for about 2 h. The mixture was cooled to ambient temperature then purified by RP-HPLC (Table 1, Method f). Concentration under reduced pressure of most of the organic solvent resulted in a precipitate which was collected by filtration and dried to give the title compound (0.018 g, 4%): LC/MS (Table 1, Method b) Rt=1.96 min; MS m/z: 357.2 (M+H)+.

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. customthen purified by RP-HPLC (Table 1, Method f)
  3. concentrationConcentration under reduced pressure of most of the organic solvent
  4. customresulted in a precipitate which
  5. filtrationwas collected by filtration
  6. customdried