Hydrazine → HCID 71258151、化合物
反応式
[S:1]([C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][CH:14]=1)[C:8](OC)=[O:9])(=[O:4])(=[O:3])[NH2:2].[NH2:15][NH2:16]>CO>[NH:15]([C:8]([C:7]1[CH:6]=[C:5]([S:1]([NH2:2])(=[O:4])=[O:3])[CH:14]=[CH:13][CH:12]=1)=[O:9])[NH2:16]参加物
4
反応条件
- 温度
- 65 °C
実験手順
Methyl 3-sulfamoylbenzoate (110 mg, 0.511 mmol) was added to the hydrazine (32.8 mg, 1.022 mmol) in methanol and refluxed for 8 h at 65° C. Following cooling, reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and then compound was purified by flash chromatography (5% methanol/DCM) to yield the 3-(hydrazinecarbonyl)benzenesulfonamide (57 mg, 0.260 mmol, 50.8% yield) as a white solid. 1H NMR (CD3OD, 400 MHz): δ 8.32 (m, 1H), 8.04 (d, 1H, J=7.6 Hz), 7.97 (d, 1H, J=7.6 Hz), 7.63 (t, 1H, J=8.0 Hz). Mass [M+H]+:216.0
後処理
- temperatureFollowing cooling
- customreaction
- customAfter completion of the reaction
- customthe solvent was removed by vacuum
- customcompound was purified by flash chromatography (5% methanol/DCM)
出典と根拠
- ORDレコード
- ord-1284525798bd4ea7aea67168f1706239
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987335B2
反応ノート
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