Glyoxal → HCID 20387469, 화합물

HRID 46479노트

반응식

HRID 46479 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 20387469HCID 20387469, 화합물

시약·촉매·용매 2

HCID 80711,2-Dimethoxyethane용매HCID 8471Triethylamine용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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°

출처 및 근거

ORD 기록
ord-2d9a78c7214d496faf24eaee907671cb
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04173645

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