Hydrazine hydrate (1:1) → 3-chloro-4-cyclobutyl-6-hydrazinylPyridazine
反応式
[Cl:1][C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][C:7]=1[CH:8]1[CH2:11][CH2:10][CH2:9]1.O.[NH2:14][NH2:15]>O1CCOCC1>[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:14][NH2:15])=[CH:6][C:7]=1[CH:8]1[CH2:11][CH2:10][CH2:9]1参加物
4
実験手順
3,6-Dichloro-4-cyclobutylpyridazine (22.5 g, 0.11 mol) and hydrazine hydrate (34 ml, 0.66 mol) were heated at reflux in dioxane (280 ml) for 24 hours. Upon cooling the desired isomer crystallized from the reaction and was collected by filtration (13.3 g, 64%). 1H NMR (250 MHz , d6-DMSO) 1.68-1.86 (1H, m), 2.00-2.11 (3H, m), 2.29-2.38 (2H, m), 3.52-3.61 (1H, m), 4.35 (2H, br), 6.99 (1H, s), 8.06 (1H, br); MS (ES+) m/e 198 [MH]+, 200 [MH]+.
後処理
- temperatureUpon cooling the desired isomer
- customcrystallized from the reaction
- filtrationwas collected by filtration (13.3 g, 64%)
出典と根拠
- ORDレコード
- ord-ee749b0974f94195a9d027d4446f3588
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06303605B1
反応ノート
読み込み中…