Triethylamine → 4-Benzothiazol-2-YL-2-methyl-2H-pyrazol-3-ylamine
反応式
[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]参加物
5
実験手順
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%).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-3aef9b3217984743b60618149830d0ee
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434720B2
反応ノート
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