Methylmalonic Acid → 1,3,5-Trimethyl-2,4,6(1H,3H,5H)-pyrimidinetrione

HRID 463294

반응식

HRID 463294 반응식
[CH3:1][NH:2][C:3]([NH:5][CH3:6])=[O:4].[CH3:7][CH:8]([C:12]([OH:14])=O)[C:9]([OH:11])=O.C(OC(=O)C)(=O)C>C(O)(=O)C>[CH3:1][N:2]1[C:9](=[O:11])[CH:8]([CH3:7])[C:12](=[O:14])[N:5]([CH3:6])[C:3]1=[O:4]

참가 물질

5

반응물 3

HCID 487Methylmalonic AcidHCID 7293N,N'-DimethylureaHCID 7918Acetic Anhydride

생성물 1

HCID 818201,3,5-Trimethyl-2,4,6(1H,3H,5H)-pyrimidinetrione수율 42%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
90 °C

실험 절차

75 g (0.85 mol) of 1,3-dimethylurea and 102 g (0.86 mol) of methyl malonic acid were dissolved in 300 ml of glacial acetic acid at 65° C. To the solution was added 330 ml of acetic anhydride, the temperature was gradually raised and the mixture was refluxed by heating at 90° C. for 6 hours. The reaction solution was concentrated under reduced pressure, and benzene was added to the residue. The crystals thus-deposited were collected by filtration and recrystallized from benzene to obtain 60 g of 1,3,5-trimethylbarbituric acid. Yield: 42%, Melting Point: 83° to 85° C.

후처리

  1. temperaturethe temperature was gradually raised
  2. temperaturethe mixture was refluxed
  3. concentrationThe reaction solution was concentrated under reduced pressure, and benzene
  4. additionwas added to the residue
  5. filtrationThe crystals thus-deposited were collected by filtration
  6. customrecrystallized from benzene

출처 및 근거

ORD 기록
ord-f269a157919840d7a4b8c7fd091a9142
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04518685

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