Hydrazine → 3-(Morpholine-4-sulfonyl)benzohydrazide

HRID 1777015

반응식

HRID 1777015 반응식
[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=2)[C:13](OC)=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1.[NH2:20][NH2:21]>CO>[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=2)[C:13]([NH:20][NH2:21])=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 779656Methyl 3-(morpholinosulfonyl)benzoate

생성물 1

HCID 8772463-(Morpholine-4-sulfonyl)benzohydrazide

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
65 °C

실험 절차

Methyl 3-(morpholinosulfonyl)benzoate (120 mg, 0.421 mmol) was added to hydrazine (17.52 mg, 0.547 mmol) in methanol and refluxed for 12 h at 65° C. The reaction was monitored by TLC. Upon completion of the reaction and cooling the reaction mixture, the solvent was removed by vacuum and then compound was purified by column chromatography to yield the title compound as an off white solid (90 mg). 1H NMR (400 MHz, CDCl3): δ 8.16 (m, 1H), 8.12 (m, 1H), 8.04 (m, 1H), 7.85 (m, 1H), 7.63 (t, 1H, J=8.0 Hz), 4.19 (m, 2H), 3.71 (m, 4H), 2.97 (m, 4H). ESI-MS: 286.1 [M+H]+.

후처리

  1. customUpon completion of the reaction
  2. temperaturecooling the reaction mixture
  3. customthe solvent was removed by vacuum
  4. customcompound was purified by column chromatography

출처 및 근거

ORD 기록
ord-d13c493a79f245d6bfe9765152d75767
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09266838B2

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