Ammonia → 6-(2-Chloro-benzoimidazol-1-yl)-pyrimidin-4-ylamine
반응식
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[C:11](Cl)[N:10]=[CH:9][N:8]=2)[C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=2[N:3]=1.[NH3:18]>CC(O)C>[Cl:1][C:2]1[N:6]([C:7]2[N:8]=[CH:9][N:10]=[C:11]([NH2:18])[CH:12]=2)[C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=2[N:3]=1참가 물질
4
반응 조건
- 온도
- 50 °C
실험 절차
A mixture of 2-Chloro-1-(6-chloro-pyrimidin-4-yl)-1H-benzoimidazole (500 mg, 1.89 mmol) and 10 mL 2 M Ammonia in 2-propanol is heated at 50° C. in a sealed tube for overnight. The reaction mixture is then cooled to room temperature, concentrated and treated with 10 mL H2O. The solid is collected by filtration and washed with water, dried to afford the title compound as a solid: 1H NMR 400 MHz (DMSO-d6) δ 8.50 (s, 1H), 7.72-7.67 (m, 1H), 7.60-7.55 (m, 1H), 7.44 (s, 2H), 7.37-7.31 (m, 2H), 6.71 (dd, J=1.2 Hz, 1H); MS m/z 246.1 (M+1).
후처리
- temperatureThe reaction mixture is then cooled to room temperature
- concentrationconcentrated
- additiontreated with 10 mL H2O
- filtrationThe solid is collected by filtration
- washwashed with water
- customdried
출처 및 근거
- ORD 기록
- ord-ce7c115d59364da58cd817432fa1063d
- 출처 데이터셋
- uspto-grants-2013_04
- 특허 번호
- US08426404B2
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