Ethanol → 6-(3,4-dimethoxyphenyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione

HRID 65143

반응식

HRID 65143 반응식
[C:1]([CH2:13][C:14]([O:16]CC)=O)(=O)[C:2]1[CH:11]=[CH:10][C:7]([O:8][CH3:9])=[C:4]([O:5][CH3:6])[CH:3]=1.[CH3:19][NH:20][C:21]([NH:23][CH3:24])=[O:22].C(O)C>Cl.O>[CH3:6][O:5][C:4]1[CH:3]=[C:2]([C:1]2[N:23]([CH3:24])[C:21](=[O:22])[N:20]([CH3:19])[C:14](=[O:16])[CH:13]=2)[CH:11]=[CH:10][C:7]=1[O:8][CH3:9]

참가 물질

6

반응물 3

HCID 702EthanolHCID 7293N,N'-DimethylureaHCID 2758465Ethyl 3,4-dimethoxybenzoylacetate

생성물 1

HCID 140964656-(3,4-dimethoxyphenyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione수율 69.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매2회HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

To a mixture of ethyl veratroylacetate (10 g) and N,N'-dimethylurea (3.84 g) were added conc. hydrochloric acid (1 drop) and ethanol (1 ml). The mixture was heated at 120° C. for 3.5 hours under reduced pressure. To the residue was added another conc. hydrochloric acid (2 drops) and the mixture was heated again at 120° C. for 4 hours under reduced pressure. To the reaction mixture was added water and extracted with ethyl acetate. The extract was dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated with a mixture of isopropyl ether and ethyl acetate to give 6-(3,4-dimethoxyphenyl)-1,3-dimethyl-2,4(1H,3H)pyrimidinedione (7.60 g).

후처리

  1. temperaturethe mixture was heated again at 120° C. for 4 hours under reduced pressure
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over magnesium sulfate
  4. customevaporated under reduced pressure
  5. customThe residue was triturated with a mixture of isopropyl ether and ethyl acetate

출처 및 근거

ORD 기록
ord-46819ab8a80f48119baf7d619bb8feff
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04612376

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