反応 #156346

反応方程式

6-(1-Methyl-1H-pyrazol-4-yl)-pyridazin-3-ylamine

Chloroacetaldehyde

H2O

NaHCO3

→

title compound

6-(1-Methyl-1H-pyrazol-4-yl)-imidazo[1,2-b]pyridazine

溶媒

EtOH

反応条件

後処理

1. 1
   その他The solvent was removed
2. 2
   workup.ADDITIONa solution of 5% NaHCO3 was added
3. 3
   抽出The mixture was extracted twice with DCM/MeOH (9/1)
4. 4
   洗浄The combined organic phases were washed with brine
5. 5
   乾燥dried over Na2SO4
6. 6
   その他the solvent was removed

実験手順

6-(1-Methyl-1H-pyrazol-4-yl)-pyridazin-3-ylamine (Stage 8.3, 2.41 g, 13.8 mmol) was dissolved in EtOH (18 mL). Chloroacetaldehyde 55% in H2O (1.61 mL, 13.8 mmol) and NaHCO3 (2.3 g, 27.5 mmol) were added. The RM was stirred at 80° C. for 5 h. The solvent was removed and a solution of 5% NaHCO3 was added. The mixture was extracted twice with DCM/MeOH (9/1). The combined organic phases were washed with brine, dried over Na2SO4, and the solvent was removed to afford the title compound as a black solid (tR 1.0 min (conditions 2), MH+=200).

出典