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

HRID 255728
ノート
印刷プレビュー

反応式

HRID 255728 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f304a988f106450d991ff6dd6ce7b1c8
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04698340

反応ノート

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