Cyclopropylamine → 5-Chloro-N3-cyclopropylpyridazine-3,4-diamine
反応式
Cl[C:2]1[N:3]=[N:4][CH:5]=[C:6]([Cl:9])[C:7]=1[NH2:8].[CH:10]1([NH2:13])[CH2:12][CH2:11]1>>[Cl:9][C:6]1[C:7]([NH2:8])=[C:2]([NH:13][CH:10]2[CH2:12][CH2:11]2)[N:3]=[N:4][CH:5]=1参加物
3
反応条件
- 温度
- 120 °C
実験手順
3,5-Dichloro-4-aminopyridazine (5.12 g, 31.2 mmol) was added to cyclopropylamine (37.0 g, 650 mmol) in a stainless steel sealed container (100 mL capacity), to give a homogenous solution. The mixture was heated for 12 hours at 120° C. The reaction mixture was cooled to room temperature then evaporated in vacuo. The residue was dissolved in EtOAc (150 mL) with sonication and stirring. The EtOAc solution was washed with 10% aqueous potassium carbonate solution (2×200 mL), dried over anhydrous MgSO4, then filtered and evaporated in vacuo. The mixture was redissolved in CH2Cl2 and purified using silica gel column chromatography eluting with CH2Cl2 (100 mL), then EtOAc (150 mL) to give the title compound as a light orange solid in 73% yield, 4.2 g.