Water → HCID 178508281, 화합물
반응식
[C:1]1([C:7]2[N:8]=[C:9]([NH:12]C(=O)C)[NH:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.OS(O)(=O)=O>CO>[C:1]1([C:7]2[N:8]=[C:9]([NH2:12])[NH:10][CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1참가 물질
5
실험 절차
To a solution of the above 0.5 g (2.4 mmol) N-(4-phenyl-1H-imidazol-2-yl)-acetamide in MeOH (20 mL) was added water (20 mL) and conc. H2SO4 (1 mL). The mixture was refluxed under nitrogen for 2 days. After cooling to rt, the organic solvent was removed under vacuum. The reaction mixture was neutralized with saturated sodium bicarbonate aq. solution (50 mL) and extracted with ethyl acetate (150 mL). The organic layer was dried and condensed. The residue was purified by a flash column chromatography eluting with EtOAc then EtOAc/MeOH=7:1 to give 4-phenyl-1H-imidazol-2-ylamine (160 mg, 41%). LCMS: 160 (M+1)+.
후처리
- temperatureThe mixture was refluxed under nitrogen for 2 days
- customthe organic solvent was removed under vacuum
- extractionextracted with ethyl acetate (150 mL)
- customThe organic layer was dried
- customcondensed
- customThe residue was purified by a flash column chromatography
- washeluting with EtOAc
출처 및 근거
- ORD 기록
- ord-843d07bf7f5a4b908f8d2acca3f33335
- 출처 데이터셋
- uspto-grants-2013_12
- 특허 번호
- US08598353B2
반응 노트
불러오는 중…