HRID226073

反应详情

EQUATION

反应方程式

HRID 226073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

190 mg of 3-Bromo-2-methyl-thieno[2,3-c]pyridine (0.83 mmol) is placed into the vial with 1.78 ml of Reiki Zn, suspension in THF (1.25 mmol) and capped and heated at 100° C. for 2 h. The excess Zinc is allowed to settle down and the solution is transferred to the vial containing 172 mg of 8-(1-ethyl-propyl)-3-iodo-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.5 mmol) and 24 mg of PdCl2(pddf) (0.03 mmol) in 3 ml of dry THF. The vial is capped with a Teflon cap and heated at 80° C. overnight. The reaction mixture is quenched with sat. NH4Cl, extracted with CH2Cl2, dried over Na2SO4 and evaporated. The crude product is applied onto a silica-gel chromatography column (Hexane:AcOEt:2 M NH3 in MeOH=20:5:1) to give 28 mg of the title compound. Yield 15%. mass spectrum (m/e): 365 (M+1).

WORKUP

后处理

  1. customcapped
  2. customcap
  3. temperatureheated at 80° C. overnight
  4. customThe reaction mixture is quenched with sat. NH4Cl
  5. extractionextracted with CH2Cl2
  6. dry with materialdried over Na2SO4
  7. customevaporated