Ethanol → 7-(4-(4-Chlorobenzoyl)benzyl)-2,6-diethoxypurine

HRID 1291205ノート

反応式

HRID 1291205 の反応式
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([C:6]([C:8]2[CH:25]=[CH:24][C:11]([CH2:12][N:13]3[C:21]4[C:16](=[N:17][C:18](Cl)=[N:19][C:20]=4Cl)[N:15]=[CH:14]3)=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.[O-:28][CH2:29][CH3:30].[Na+].[CH2:32]([OH:34])[CH3:33]>O>[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([C:6]([C:8]2[CH:9]=[CH:10][C:11]([CH2:12][N:13]3[C:21]4[C:16](=[N:17][C:18]([O:34][CH2:32][CH3:33])=[N:19][C:20]=4[O:28][CH2:29][CH3:30])[N:15]=[CH:14]3)=[CH:24][CH:25]=2)=[O:7])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 702EthanolHCID 2723922Sodium ethoxideHCID 189188407-(4-(4-Chlorobenzoyl)benzyl)-2,6-dichloropurine

生成物 1

HCID 189189697-(4-(4-Chlorobenzoyl)benzyl)-2,6-diethoxypurine収率 67%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 7-(4-(4-chlorobenzoyl)benzyl)-2,6-dichloropurine (1.12 g) in ethanol (30 ml) was added sodium ethoxide (1.83 g) and the mixture was stirred at room temperature for 96 hours. This reaction mixture was diluted with water and extracted with ethyl acetate. The extract was washed with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate and the solvent was distilled off. The residue was washed with ether and hexane to provide the title compound (0.78 g, 67%) as colorless powder. 1H-NMR (CDCl3) δ: 1.34(3H,t,J=7.OHz), 1.50(3H,t,J=7.OHz), 4.50(2H,q,J=7.OHz), 4.55(2H,q,J=7.OHz), 5.53(2H,s), 7.25-7.80(8H,m), 7.98(1H,s).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated aqueous NaCl solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off
  5. washThe residue was washed with ether and hexane

出典と根拠

ORDレコード
ord-9e8f4277d9f64b7f9d09d65a429406a6
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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