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

HRID 4679

반응식

HRID 4679 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-341f97577ef543daa52fec737b242a18
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727073

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