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Ethanol → Ethyl 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinylacetate

HRID 255728
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HRID 255728 반응식
[C:1]([CH2:3][C:4]1[C:5]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([N+:23]([O-:25])=[O:24])[CH:18]=2)=[N:6][C:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:8][C:9]=1[CH3:10])#N.S(=O)(=O)(O)O.[CH2:31]([OH:33])[CH3:32].C(=O)([O-])[O-:35].[Na+].[Na+]>O.C(Cl)(Cl)Cl>[CH3:10][C:9]1[N:8]=[C:7]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:6]=[C:5]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([N+:23]([O-:25])=[O:24])[CH:18]=2)[C:4]=1[CH2:3][C:1]([O:33][CH2:31][CH3:32])=[O:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 99967205-Cyanomethyl-6-methyl-2-phenyl-4-(3-nitrophenyl)pyrimidine

생성물 1

HCID 10362221Ethyl 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinylacetate

시약·촉매·용매 2

HCID 962Water
용매
HCID 6212Chloroform용매

실험 절차

A mixture of 5 -cyanomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (5 g), conc. sulfuric acid (12 g) and ethanol (50 ml) was gently refluxed for 72 hours. The reaction mixture was poured into a suspension of chloroform (200 ml) and water (100 ml), and then adjusted to pH 8.5 with 10% aqueous sodium carbonate solution. The separated organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and evaporated in vacuo. The residual substance was recrystallized from diethyl ether-n-hexane to give ethyl 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinylacetate (3.7 g).

후처리

  1. temperaturewas gently refluxed for 72 hours
  2. washThe separated organic layer was washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residual substance was recrystallized from diethyl ether-n-hexane

출처 및 근거

ORD 기록
ord-f304a988f106450d991ff6dd6ce7b1c8
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04698340

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