Dimethylformamide dimethyl acetal → HCID 178484240、化合物
反応式
[NH2:1][C:2]1[N:3]=[N:4][C:5]([Br:8])=[CH:6][CH:7]=1.CO[CH:11](OC)[N:12]([CH3:14])[CH3:13]>>[Br:8][C:5]1[N:4]=[N:3][C:2](/[N:1]=[CH:11]/[N:12]([CH3:14])[CH3:13])=[CH:7][CH:6]=1参加物
3
実験手順
3-Amino-6-bromopyridazine (5.0 g, 28.7 mmol) was heated and stirred with dimethylformamide dimethylacetal (5.36 g, 6.0 mL, 45.0 mmol) under nitrogen at 110° C. for 3 h. The brown homogeneous reaction mixture was cooled to room temperature. The resulting heterogeneous slurry was stirred in EtOAc/hexanes (1:1, 75 mL) and filtered. The filtered solid was suction dried to obtain apparently (E)-N′-(6-bromopyridazin-3-yl)-N,N-dimethylformimidamide (4.9 g) as a pale pink crystalline solid. 1H NMR (300 MHz, DMSO-d6) δ 8.45 (s, 1H), 7.64 (d, J=9.1 Hz, 1H), 7.03 (d, J=9.1 Hz, 1H), 3.11 (s, 3H), 3.00 (s, 3H).
後処理
- filtrationfiltered
- customdried
出典と根拠
- ORDレコード
- ord-3a6bfbd691de477abcfc45c000071a63
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09145433B2
反応ノート
読み込み中…