Hydrochloric Acid → HCID 61609705, 화합물
반응식
[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]참가 물질
7
실험 절차
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).
후처리
- temperatureThe solution was refluxed for 24 h
- temperaturecooled
- filtrationThe precipitate was filtered
- washwashed with water
출처 및 근거
- ORD 기록
- ord-4312f3a09a094b899151e2b6289e4bd2
- 출처 데이터셋
- uspto-grants-2013_12
- 특허 번호
- US08604023B2
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