Potassium Carbonate → 2,2-Dimethylpropionic acid [8-chloro-3-(2,2-dimethylpropionyloxymethyl)-7-(3-methylbut-2-enyl)-2,6-dioxo-2,3,6,7-tetrahydropurin-1-yl]methyl ester

HRID 1792057ノート

反応式

HRID 1792057 の反応式
[Cl:1][C:2]1[NH:10][C:9]2[C:8](=[O:11])[N:7]([CH2:12][O:13][C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[C:6](=[O:20])[N:5]([CH2:21][O:22][C:23](=[O:28])[C:24]([CH3:27])([CH3:26])[CH3:25])[C:4]=2[N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:36][CH:37]=[C:38]([CH3:40])[CH3:39]>CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[N:10]([CH2:36][CH:37]=[C:38]([CH3:40])[CH3:39])[C:9]2[C:8](=[O:11])[N:7]([CH2:12][O:13][C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[C:6](=[O:20])[N:5]([CH2:21][O:22][C:23](=[O:28])[C:24]([CH3:27])([CH3:26])[CH3:25])[C:4]=2[N:3]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 700922-Butene, 1-bromo-3-methyl-HCID 235368892,2-Dimethylpropionic acid [8-chloro-3-(2,2-dimethylpropionyloxymethyl)-2,6-dioxo-2,3,6,7-tetrahydropurin-1-yl]methyl ester

生成物 1

HCID 235368912,2-Dimethylpropionic acid [8-chloro-3-(2,2-dimethylpropionyloxymethyl)-7-(3-methylbut-2-enyl)-2,6-dioxo-2,3,6,7-tetrahydropurin-1-yl]methyl ester

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2,2-Dimethylpropionic acid [8-chloro-3-(2,2-dimethylpropionyloxymethyl)-2,6-dioxo-2,3,6,7-tetrahydropurin-1-yl]methyl ester (600 mg) and potassium carbonate (630 mg) were suspended in N,N-dimethylformamide (10 ml), and 4-bromo-2-methyl-2-butene (183 μl) was added to the suspension at room temperature. After the reaction mixture was stirred at room temperature for 24 hours, the mixture was diluted with ethyl acetate, washed with water, and dried over anhydrous magnesium sulfate. After the solvent was removed by distillation from the organic layer, the residue was purified by silica gel column chromatography to give 470 mg of the title compound from the elution fraction of hexane-ethyl acetate (3:1).

後処理

  1. washwashed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customAfter the solvent was removed by distillation from the organic layer
  4. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-29e4af81ff0c42398af262e4cec2dd03
出典データセット
uspto-grants-2006_07
特許番号
US07074798B2

反応ノート

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