HRID1675105

反应详情

EQUATION

反应方程式

HRID 1675105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

DIPEA (12.15 mL, 69.78 mmol) was added to 6-chloro-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine (10.35 g, 46.52 mmol) and 1-(4-hydroxyphenyl)piperazine (CAS 56621-48-8, 9.12 g, 51.17 mmol) in DMF (80 mL). The resulting solution was stirred at 80° C. for 1 hour. The reaction mixture was cooled to room temperature, evaporated to dryness and the residue re-dissolved in DCM (250 mL). The solution was washed with water (200 mL), dried over MgSO4 and evaporated to afford crude product, which was triturated with diethyl ether. The resulting solid was collected by filtration and dried under vacuum to give 4-[4-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperazin-1-yl]phenol (14.27 g, 84%) as a solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customevaporated to dryness
  3. dissolutionthe residue re-dissolved in DCM (250 mL)
  4. washThe solution was washed with water (200 mL)
  5. dry with materialdried over MgSO4
  6. customevaporated
  7. customto afford crude product, which
  8. customwas triturated with diethyl ether
  9. filtrationThe resulting solid was collected by filtration
  10. customdried under vacuum