Uracil → 1-Benzyloxycarbonylmethyl-2,4-dioxopyrimidine

HRID 2308182ノート

反応式

HRID 2308182 の反応式
CN(C)C=O.[O:6]=[C:7]1[NH:12][C:11](=[O:13])[CH:10]=[CH:9][NH:8]1.Br[CH2:15][C:16]([O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17].C(=O)([O-])[O-].[K+].[K+]>O>[CH2:19]([O:18][C:16]([CH2:15][N:8]1[CH:9]=[CH:10][C:11](=[O:13])[NH:12][C:7]1=[O:6])=[O:17])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

参加物

6

反応物 4

HCID 1174UracilHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 62576Benzyl bromoacetate

生成物 1

HCID 226011191-Benzyloxycarbonylmethyl-2,4-dioxopyrimidine収率 60.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To anhydrous dimethylformamide solution (10 ml) containing 2,4-dioxopyrimidine (1.0 g) are added benzyl bromoacetate (2.5 g) and potassium carbonate (2.5 g), and the mixture is stirred at room temperature for 15 hours. The reaction solution is poured into water, and the mixture is extracted with ethyl acetate. The extract is washed with a saturated brine, and dried over anhydrous magnesium sulfate. The solvent is removed by evaporation under reduced pressure, and the precipitated crystals are washed with diethyl ether to give the desired 1-benzyloxycarbonylmethyl-2,4-dioxopyrimidine (1.4 g) as colorless crystals.

後処理

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe extract is washed with a saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent is removed by evaporation under reduced pressure
  5. washthe precipitated crystals are washed with diethyl ether

出典と根拠

ORDレコード
ord-ddd691a8b02340e7a32db9bdb3211bb4
出典データセット
uspto-grants-2004_12
特許番号
US06835714B1

反応ノート

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