3-Sulfolene → 1-(1,1-Dioxothiolan-3-yl)-1-phenylhydrazine

HRID 900026

반응식

HRID 900026 반응식
[S:1]1([CH2:7][CH:6]=[CH:5][CH2:4]1)(=[O:3])=[O:2].[C:8]1([NH:14][NH2:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[OH-].[K+]>>[C:8]1([N:14]([CH:5]2[CH2:6][CH2:7][S:1](=[O:3])(=[O:2])[CH2:4]2)[NH2:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

4

반응물 3

HCID 64983-SulfoleneHCID 7516PhenylhydrazineHCID 14797Potassium Hydroxide

생성물 1

HCID 28017481-(1,1-Dioxothiolan-3-yl)-1-phenylhydrazine수율 53%

반응 조건

온도
60 °C

실험 절차

Butadiene sulfone (0.5 mol, obtained from Aldrich chemicals, Milwaukee, Wis.) and phenyl hydrazine (0.55 mol, 1.1 equiv. obtained from Aldrich Chemicals, Milwaukee, Wis.) were stirred for 5-10 minutes, and then 40% aqueous KOH solution (0.005 mol, 0.01 equiv. obtained from Aldrich Chemicals, Milwaukee, Wis.)) was added. The mixture was heated at 60° C. for 2 hours whereupon a solid separated. After 10 hours at room temperature, the solid was filtered, washed with excess of water and recrystallized from methanol to give the product as white crystals; yield 53%; mp 119.9-121.5° C.; 1H-NMR and 13C-NMR spectra in CDCl3 were in full agreement with the structure.

후처리

  1. customseparated
  2. filtrationthe solid was filtered
  3. washwashed with excess of water
  4. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-bbeafbfc484a4ef9983909737ecb41ef
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07358014B2

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