HRID226081

反应详情

EQUATION

反应方程式

HRID 226081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

214 mg of 3-Bromo-thieno[2,3-b]pyridine (1.0 mmol) is dissolved in 1.5 ml of dry THF and cooled to −78° C. 0.44 ml of n-butyl lithium 2.5M in hexane is added slowly and stirred at −78° C. for 10 min. 2.2 ml of 0.5 M ZnCl2 in THF (1.1 mmol) is added and stirred at room temperature for 20 min. 274 mg of 8-(1-ethyl-propyl)-3-iodo-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.8 mmol) and 33 mg of PdCl2(dppf) (0.04 mmol) are added. The reaction vial is capped and heated at 80° C. for 3 days. The reaction is filtered and applied onto a silica-gel chromatography column (Hexane: AcOEt=8:1) to give 49 mg of the 3-(3-bromo-thieno[2,3-b]pyridin-2-yl)-8-(1-ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazine (11%) and 33 mg of reduced compound, 8-(1-ethyl-propyl)-2,6-dimethyl-3-thieno[2,3-b]pyridin-2-yl-imidazo[1,2-b]pyridazine, (9%).

WORKUP

后处理

  1. stirringstirred at room temperature for 20 min
  2. customThe reaction
  3. customvial is capped
  4. temperatureheated at 80° C. for 3 days
  5. filtrationThe reaction is filtered