Glyoxal → HCID 20387469、化合物

HRID 46479ノート

反応式

HRID 46479 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10]([NH:12][CH3:13])=[S:11])[CH3:2].[CH:14]([CH:16]=[O:17])=[O:15].NC(N)=S>C(COC)OC.C(N(CC)CC)C>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH:14]([OH:15])[CH:16]([OH:17])[N:12]([CH3:13])[C:10]1=[S:11])[CH3:2]

参加物

6

反応物 3

HCID 7860GlyoxalHCID 2723790ThioureaHCID 4105389N-(2-Ethylphenyl)-N'-methylthiourea

生成物 1

HCID 20387469HCID 20387469、化合物

試薬・触媒・溶媒 2

HCID 80711,2-Dimethoxyethane溶媒HCID 8471Triethylamine溶媒

反応条件

温度
50 °C

実験手順

30.0 g of N-(2-ethyl-phenyl)-N'-methyl-thiourea were stirred in 200 ml of dimethoxyethane and 10 ml of triethylamine, and 36.0 g of a 30% strength aqueous glyoxal solution were added. The mixture was stirred for 1 hour at 20° C. and for 1 hour at 50° C., the thiourea dissolving completely. The solvent was distilled off in vacuo, the residue was stirred with water and a little dilute acetic acid and the oily reaction product was taken up in methylene chloride. The methylene chloride solution was washed with water, dried over potassium carbonate, concentrated and completely freed from the solvent at 60°/1.0 mm Hg. This gave 26.0 g of the reaction product as a viscous oil which slowly solidified. The elementary analysis and the NMR spectra were in agreement with the supposed structure.

後処理

  1. distillationThe solvent was distilled off in vacuo
  2. stirringthe residue was stirred with water
  3. washThe methylene chloride solution was washed with water
  4. dry with materialdried over potassium carbonate
  5. concentrationconcentrated
  6. customcompletely freed from the solvent at 60°

出典と根拠

ORDレコード
ord-2d9a78c7214d496faf24eaee907671cb
出典データセット
uspto-grants-1979_11
特許番号
US04173645

反応ノート

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