6-Amino-3-chloropyridazine → HCID 178484245、化合物
反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][CH:3]=1.CO[CH:11](OC)[N:12]([CH3:14])[CH3:13]>>[Cl:1][C:2]1[N:7]=[N:6][C:5](/[N:8]=[CH:11]/[N:12]([CH3:14])[CH3:13])=[CH:4][CH:3]=1参加物
3
反応条件
- 温度
- 110 °C
実験手順
A 500 mL RB flask was charged with 6-chloropyridazin-3-amine (10.0 g, 77.2 mmol) and dimethoxy-N,N-dimethylmethanamine (206 ml, 1544 mmol), equipped with a reflux condenser, then heated to 110° C. for 3 hours then left at room temperature for 16 hours. The precipitate was collected by filtration. The mother liqour was concentrated down to give an yellow solid, which was triturated with EtOAc and collected. The solids were combined to give (E)-N′-(6-chloropyridazin-3-yl)-N,N-dimethylformamidine (11.81 g, 82.9% yield) as a white solid
後処理
- customequipped with a reflux condenser
- filtrationThe precipitate was collected by filtration
- concentrationThe mother liqour was concentrated down
- customto give an yellow solid, which
- customwas triturated with EtOAc
- customcollected
出典と根拠
- ORDレコード
- ord-f47ed11a07204948b95a84095b32d6f5
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524900B2
反応ノート
読み込み中…