Potassium Carbonate → [7-(2-Butynyl)-1-methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl 2,2-dimethylpropionate

HRID 1792055ノート

反応式

HRID 1792055 の反応式
[CH3:1][N:2]1[C:10](=[O:11])[C:9]2[NH:8][CH:7]=[N:6][C:5]=2[N:4]([CH2:12][O:13][C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[C:3]1=[O:20].C(=O)([O-])[O-].[K+].[K+].[CH2:27](Br)[C:28]#[C:29][CH3:30]>CN(C)C=O.C(OCC)(=O)C>[CH2:27]([N:8]1[C:9]2[C:10](=[O:11])[N:2]([CH3:1])[C:3](=[O:20])[N:4]([CH2:12][O:13][C:14](=[O:19])[C:15]([CH3:16])([CH3:17])[CH3:18])[C:5]=2[N:6]=[CH:7]1)[C:28]#[C:29][CH3:30]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 27568621-Bromo-2-butyneHCID 23536866[1-Methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl 2,2-dimethylpropionate

生成物 1

HCID 23536882[7-(2-Butynyl)-1-methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl 2,2-dimethylpropionate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2,2-Dimethylpropionic acid [1-methyl-2,6-dioxo-1,2,6,7-tetrahydropurin-3-yl]methyl ester (1.871 g) was dissolved in N,N-dimethylformamide (30 ml), potassium carbonate (1.5 g) and 2-butynyl bromide (0.7 ml) were added to the solution, and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate, and washed with water and 1N hydrochloric acid. The organic layer was dried over anhydrous magnesium sulfate and filtered. Then, the solvent was removed by distillation. The residue was purified by silica gel column chromatography to give 2.12 g of the title compound from the elution fraction of hexane-ethyl acetate (3:2).

後処理

  1. washwashed with water and 1N hydrochloric acid
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customThen, the solvent was removed by distillation
  5. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-375bbb219b1e45e280b6eb86b75a52a1
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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