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

HRID 877610노트

반응식

HRID 877610 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 (s, 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-801770c7005246b4ac17748c4cdd1d00
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987335B2

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