Water → 1-(4-chlorobutyl)-5-methylpyrimidine-2,4(1H,3H)-dione

HRID 1640457

反応式

HRID 1640457 の反応式
[OH:1][C:2]1[C:7]([CH3:8])=[CH:6][NH:5][C:4](=[O:9])[N:3]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:17][CH2:18][CH2:19][CH2:20][Cl:21].O>CS(C)=O>[Cl:21][CH2:20][CH2:19][CH2:18][CH2:17][N:5]1[CH:6]=[C:7]([CH3:8])[C:2](=[O:1])[NH:3][C:4]1=[O:9]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 813641-Bromo-4-chlorobutaneHCID 178430899HCID 178430899、化合物

生成物 1

HCID 593375871-(4-chlorobutyl)-5-methylpyrimidine-2,4(1H,3H)-dione収率 41%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

10.1 g (80.0 mmol) of 4-hydroxy-5-methylpyrimidin-2(1H)-one (thymine) in 300 ml of dimethyl sulfoxide (DMSO) and 11.1 g (80.0 mmol) of K2CO3 were stirred at room temperature for 1 hour. Then 13.7 g (80.0 mmol) of 1-bromo-4-chlorobutane were added dropwise to the mixture, and the reaction mixture was then stirred at room temperature for 5 hours. Water was added to the reaction mixture, and it was then extracted with ethyl acetate. The aqueous phase was then neutralized and extracted with methylene chloride. Drying of the organic phase, removal of the desiccant by filtration and evaporation of the solvent to dryness in vacuo resulted in 7.1 g of the title compound

後処理

  1. extractionwas then extracted with ethyl acetate
  2. extractionextracted with methylene chloride
  3. customDrying of the organic phase, removal of the
  4. filtrationdesiccant by filtration and evaporation of the solvent to dryness in vacuo

出典と根拠

ORDレコード
ord-b162710974be453188102109c39d2459
出典データセット
uspto-grants-2012_02
特許番号
US08114875B2

関連ノート

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