反応 #313255

反応方程式

8-(1-ethyl-propyl)-3-iodo-2,6-dimethyl-imidazo[1,2-b]pyridazine

3-Bromo-2-methyl-thieno[2,3-c]pyridine

→

title compound

収率 15.4%

8-(1-Ethyl-propyl)-2,6-dimethyl-3-(2-methyl-thieno[2,3-c]pyridin-3-yl)-imidazo[1,2-b]pyridazine

収率 15.4%

溶媒

THF

THF

反応条件

後処理

1. 1
   その他capped
2. 2
   その他cap
3. 3
   温度heated at 80° C. overnight
4. 4
   その他The reaction mixture is quenched with sat. NH4Cl
5. 5
   抽出extracted with CH2Cl2
6. 6
   乾燥dried over Na2SO4
7. 7
   その他evaporated

実験手順

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).

出典