Triethylamine → Ethyl 2-methyl-4-(3,4-dimethoxyphenyl)-5-pyrimidinecarboxylate

HRID 4679

反応式

HRID 4679 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[C:6]([C:8](=[CH:14]N(C)C)[C:9]([O:11][CH2:12][CH3:13])=[O:10])=O.Cl.[C:24]([NH2:27])(=[NH:26])[CH3:25].C(N(CC)CC)C>C(O)C>[CH3:25][C:24]1[N:27]=[C:6]([C:5]2[CH:18]=[CH:19][C:20]([O:21][CH3:22])=[C:3]([O:2][CH3:1])[CH:4]=2)[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:14][N:26]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 67170Acetamidine monohydrochlorideHCID 53710889Ethyl 2-(3,4-dimethoxybenzoyl)-2-(dimethylaminomethylene)acetate

生成物 1

HCID 20151431Ethyl 2-methyl-4-(3,4-dimethoxyphenyl)-5-pyrimidinecarboxylate収率 45.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of ethyl 2-(3,4-dimethoxybenzoyl)-2-(dimethylaminomethylene)acetate (31 g), acetoamidine hydrochloride (13.3 g) and triethylamine (16.2 g) in ethanol (200 ml) was refluxed for 10 hours under stirring. The reaction mixture was evaporated in vacuo and the residue was dissolved in a mixture of ethyl acetate and water. The separatedorganic layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was crystallized from ethyl ether to give ethyl 2-methyl-4-(3,4-dimethoxyphenyl)-5-pyrimidinecarboxylate (14 g).

後処理

  1. customThe reaction mixture was evaporated in vacuo
  2. dissolutionthe residue was dissolved in a mixture of ethyl acetate and water
  3. washThe separatedorganic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was crystallized from ethyl ether

出典と根拠

ORDレコード
ord-341f97577ef543daa52fec737b242a18
出典データセット
uspto-grants-1988_02
特許番号
US04727073

関連ノート

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