Dimethylformamide → 5-Bromo-2-(2,2-diethoxyethoxy)pyrimidine

HRID 15063

反応式

HRID 15063 の反応式
[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][OH:6])[CH3:2].C(=O)([O-])[O-].[Cs+].[Cs+].CN(C=O)C.[Br:21][C:22]1[CH:23]=[N:24][C:25](Cl)=[N:26][CH:27]=1>O>[Br:21][C:22]1[CH:23]=[N:24][C:25]([O:6][CH2:5][CH:4]([O:7][CH2:8][CH3:9])[O:3][CH2:1][CH3:2])=[N:26][CH:27]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 121292,2-DiethoxyethanolHCID 6066655-Bromo-2-chloropyrimidine

生成物 1

HCID 684312375-Bromo-2-(2,2-diethoxyethoxy)pyrimidine収率 94.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2,2-Diethoxyethanol (1.6 g) and cesium carbonate (5.8 g) were added to DMF solution (10 mL) of 5-bromo-2-chloropyrimidine (1.15 g), and stirred at room temperature for 12 hours. After addition of water, the reaction liquid was extracted with ethyl acetate and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the residue was purified on silica gel column chromatography (C-200; ethyl acetate:hexane=1:9-1:4) to provide the title compound (1.63 g, 94%).

後処理

  1. customthe reaction liquid
  2. extractionwas extracted with ethyl acetate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationConcentrating the solvent under reduced pressure
  5. customthe residue was purified on silica gel column chromatography (C-200; ethyl acetate:hexane=1:9-1:4)

出典と根拠

ORDレコード
ord-1ba2013ec1264fe3af9606dd2c8fb343
出典データセット
uspto-grants-2010_06
特許番号
US07732456B2

関連ノート

読み込み中…