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Hydrazine → 3-(hydrazinecarbonyl)-N-methylbenzenesulfonamide

HRID 1777050
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HRID 1777050 반응식
[NH2:1][NH2:2].[CH3:3][NH:4][S:5]([C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][CH:17]=1)[C:11](OC)=[O:12])(=[O:7])=[O:6]>CO>[NH:1]([C:11]([C:10]1[CH:9]=[C:8]([S:5]([NH:4][CH3:3])(=[O:7])=[O:6])[CH:17]=[CH:16][CH:15]=1)=[O:12])[NH2:2]
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 9320906methyl 3-(N-methylsulfamoyl)benzoate

생성물 1

HCID 677513503-(hydrazinecarbonyl)-N-methylbenzenesulfonamide수율 74.3%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
65 °C

실험 절차

Hydrazine (43.3 mg, 1.352 mmol) was added to the methyl 3-(N-methylsulfamoyl)benzoate (155 mg, 0.676 mmol) in methanol and refluxed for 12 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 column chromatography to yield 3-(hydrazinecarbonyl)-N-methylbenzenesulfonamide (120 mg, 0.502 mmol, 74.3% yield). 1H NMR (CDCl3, 400 MHz): δ 8.25 (m, 1H), 8.01 (m, 2H), 7.64 (m, 2H), 4.63 (m, 1H), 4.17 (m, 2H), 2.69 (d, 3H, J=5.2 Hz). ESI-MS: 230.0 [M+H]+

후처리

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

출처 및 근거

ORD 기록
ord-054bc86bf76c4245b7d8d905f5127334
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266838B2

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