3-环丁烯砜 → 1-(1,1-Dioxothiolan-3-yl)-1-phenylhydrazine

HRID 900026

反应方程式

HRID 900026 反应方程式
[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

参与物

4

反应物 3

HCID 64983-环丁烯砜HCID 7516苯肼HCID 14797氢氧化钾

产物 1

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

反应条件

温度
60 °C

实验过程

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.

后处理

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

来源与证据

ORD记录
ord-bbeafbfc484a4ef9983909737ecb41ef
来源数据集
uspto-grants-2008_04
专利号
US07358014B2

关联笔记

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