Hydrazine → 3-(Hydrazinecarbonyl)-N,N-dimethylbenzene-1-sulfonamide

HRID 877610ノート

反応式

HRID 877610 の反応式
[CH3:1][N:2]([CH3:16])[S:3]([C:6]1[CH:7]=[C:8]([CH:13]=[CH:14][CH:15]=1)[C:9](OC)=[O:10])(=[O:5])=[O:4].[NH2:17][NH2:18]>CO>[NH:17]([C:9]([C:8]1[CH:7]=[C:6]([S:3]([N:2]([CH3:16])[CH3:1])(=[O:5])=[O:4])[CH:15]=[CH:14][CH:13]=1)=[O:10])[NH2:18]

参加物

4

反応物 2

HCID 9321HydrazineHCID 1262217Methyl 3-(dimethylsulfamoyl)benzoate

生成物 1

HCID 38489513-(Hydrazinecarbonyl)-N,N-dimethylbenzene-1-sulfonamide収率 40%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

Methyl 3-(N,N-dimethylsulfamoyl)benzoate (150 mg, 0.617 mmol) was added to hydrazine (29.6 mg, 0.925 mmol) in methanol (10 mL) and refluxed for 8 h at 65° C. Following cooling, the reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and the compound was purified by column chromatography affording the title compound (60 mg). 1H NMR (400 MHz, CDCl3): δ 8.11 (s, 1H), 8.01 (d, 1H, J=8.4 Hz), 7.92 (d, 1H, J=8.0 Hz), 7.65 (t, 1H, J=8.0 Hz), 2.73 (s, 6H). ESI-MS: 244.0 [M+H]+.

後処理

  1. temperatureFollowing cooling
  2. customAfter completion of the reaction
  3. customthe solvent was removed by vacuum
  4. customthe compound was purified by column chromatography

出典と根拠

ORDレコード
ord-801770c7005246b4ac17748c4cdd1d00
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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