반응식
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[N:11]1[CH:15]=[C:14]([CH3:16])[N:13]=[CH:12]1)[NH2:7].[N:17]#[C:18][NH2:19].Cl>C(O)C.O>[CH3:2][O:3][C:4]1[CH:5]=[C:6]([NH:7][C:18]([NH2:19])=[NH:17])[CH:8]=[CH:9][C:10]=1[N:11]1[CH:15]=[C:14]([CH3:16])[N:13]=[CH:12]1참가 물질
6
실험 절차
3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline hydrochloride (3 g, 12.52 mmol), cyanamide (0.684 g, 16.27 mmol) and hydrochloric acid (1.564 mL, 18.77 mmol) in ethanol (20 mL) were heated to reflux o.n. The reaction mixture was concentrated under reduced pressure before the residue was poured on potassium carbonate (1.730 g, 12.52 mmol) in water (60 mL) and then put in refrigerator o.n. The formed carbonate-salt was filtered off, and dried in vacuum oven o.n. The solid was washed with several portions of DCM, dried and used as such in next step (52.3%). MS (ES+) m/z 246.2 (M+H)+
후처리
- temperatureto reflux o.n
- concentrationThe reaction mixture was concentrated under reduced pressure before the residue
- filtrationThe formed carbonate-salt was filtered off
- customdried in vacuum oven o.n
- washThe solid was washed with several portions of DCM
- customdried
출처 및 근거
- ORD 기록
- ord-747b10de2d1d40299d4b993bc021f52f
- 출처 데이터셋
- uspto-grants-2012_05
- 특허 번호
- US08188101B2
연결된 노트
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