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

HRID 1777025노트

반응식

HRID 1777025 반응식
[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]

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 1262217Methyl 3-(dimethylsulfamoyl)benzoate

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
65 °C

실험 절차

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 (5, 6H). ESI-MS: 244.0 [M+H]+.

후처리

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

출처 및 근거

ORD 기록
ord-18ce74612b254928b6340d4c70e685ea
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09266838B2

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