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

HRID 900026

反応式

HRID 900026 の反応式
[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

参加物

4

反応物 3

HCID 64983-SulfoleneHCID 7516PhenylhydrazineHCID 14797Potassium Hydroxide

生成物 1

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

反応条件

温度
60 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-bbeafbfc484a4ef9983909737ecb41ef
出典データセット
uspto-grants-2008_04
特許番号
US07358014B2

関連ノート

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