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

HRID 1291205노트

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HRID 1291205 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9e8f4277d9f64b7f9d09d65a429406a6
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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