Hydrochloric Acid → HCID 61609705、化合物
反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:10][CH:11]2[CH2:13][CH2:12]2)=C([CH:9]=1)C#N.[OH-:14].[K+].Cl.C1(C)C=CC=CC=1.[CH3:24][CH2:25][OH:26]>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:10][CH:11]2[CH2:13][CH2:12]2)=[C:24]([CH:9]=1)[C:25]([OH:14])=[O:26]参加物
7
実験手順
5-Chloro-2-(cyclopropylamino)benzonitrile (4.66 g) was dissolved in a solution of KOH (4.75 g, 3.5 eq) in EtOH (12 mL) and water (2.5 mL). The solution was refluxed for 24 h, cooled, and acidified with concentrated HCl. The precipitate was filtered, washed with water, and dried by multiple concentrations from toluene delivering pure product (4.70 g, 92% yield). 1H-NMR (400 MHz, DMSO-d6) δ 7.88 (bs, 1H), 7.70 (d, 1H), 7.42 (dd, 1H), 7.09 (d, 1H), 2.47 (m, 1H), 0.78 (m, 2H), 0.45 (m, 2H).
後処理
- temperatureThe solution was refluxed for 24 h
- temperaturecooled
- filtrationThe precipitate was filtered
- washwashed with water
出典と根拠
- ORDレコード
- ord-4312f3a09a094b899151e2b6289e4bd2
- 出典データセット
- uspto-grants-2013_12
- 特許番号
- US08604023B2
反応ノート
読み込み中…