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

HRID 65143

反応式

HRID 65143 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒2 回HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-46819ab8a80f48119baf7d619bb8feff
出典データセット
uspto-grants-1986_09
特許番号
US04612376

関連ノート

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