N,N'-Dimethylurea → 1,3-Dimethylimidazolidine-2,4-dione

HRID 2080609노트

반응식

HRID 2080609 반응식
[CH:1]([CH:3]=O)=[O:2].C(N(CC)CC)C.[CH3:12][NH:13][C:14]([NH:16][CH3:17])=[O:15]>O>[CH3:12][N:13]1[CH2:3][C:1](=[O:2])[N:16]([CH3:17])[C:14]1=[O:15]

참가 물질

5

반응물 3

HCID 7293N,N'-DimethylureaHCID 7860GlyoxalHCID 8471Triethylamine

생성물 1

HCID 1234101,3-Dimethylimidazolidine-2,4-dione수율 85%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
30 °C

실험 절차

In a 1000 ml glass vessel equipped with a stirrer, thermometer, a dropping funnel and a distillation unit was charged 290 g (2.0 mol) of 40 wt % aqueous glyoxal solution. And then, triethylamine is added thereto to prepare a basic mixed solution (At this time, the solution had a pH of 9). To the mixed solution was gradually added dropwise a solution comprising 176 g (2.0 mol) of 1,3-dimethylurea and 176 ml of water while maintaining a liquid temperature to 25 to 35° C. After stirring the solution at room temperature for 3 hours, the mixture was reacted by elevating the temperature to 200° C. over 2 hours while removing triethylamine and water under normal pressure by distillation. After completion of the reaction, the obtained reaction mixture was distilled under reduced pressure (105 to 107° C./0.67 to 1.33 kPa) to obtain 217 g (Isolation yield; 85%) of 1,3-dimethylimidazolidin-2,4-dione as a pale yellowish liquid.

후처리

  1. customIn a 1000 ml glass vessel equipped with a stirrer
  2. customto prepare a basic mixed solution (At this time
  3. customthe mixture was reacted
  4. customto 200° C.
  5. customover 2 hours
  6. customwhile removing triethylamine and water under normal pressure
  7. distillationby distillation
  8. customAfter completion of the reaction
  9. customthe obtained reaction mixture
  10. distillationwas distilled under reduced pressure (105 to 107° C./0.67 to 1.33 kPa)

출처 및 근거

ORD 기록
ord-8ba7c2a8b0944e0089f35470fd41284f
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932400B2

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