Triethylamine → 4-Benzothiazol-2-YL-2-methyl-2H-pyrazol-3-ylamine
반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10](=[CH:13][N:14]([CH3:16])C)[C:11]#[N:12].C([N:19](CC)CC)C.S(O)(O)(=O)=O.CNN>CCO>[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[CH:11]=[N:12][N:14]([CH3:16])[C:13]=1[NH2:19]참가 물질
5
실험 절차
A mixture of the 2-benzothiazol-2-yl-3-dimethylaminoacrylonitrile prepared above (96 mg, 0.42 mmol) and triethylamine (0.3 mL) in EtOH (10 mL) was treated with methylhydrazine sulfate (180 mg, 1.25 mmol) and the mixture was heated to reflux for 2 days. The solution was concentrated in vacuo and the residue was purified by flash chromatography (hexanes:EtOAc=1:1) to yield 47 mg (49%) of the title compound as a yellow powder. MS (m/z, ES+): 231 (M+1, 100%).
후처리
- temperaturethe mixture was heated
- temperatureto reflux for 2 days
- concentrationThe solution was concentrated in vacuo
- customthe residue was purified by flash chromatography (hexanes:EtOAc=1:1)
출처 및 근거
- ORD 기록
- ord-8de484a7288e48d591e72b826596b71c
- 출처 데이터셋
- uspto-grants-2010_12
- 특허 번호
- US07847101B2
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