Water → 4-(5-Bromo-imidazol-1-yl)-2-chloro-pyrimidine

HRID 1784384ノート

反応式

HRID 1784384 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].[Br:15][C:16]1[NH:20][CH:19]=[N:18][CH:17]=1.O>CN(C=O)C>[Br:15][C:16]1[N:20]([C:6]2[CH:5]=[CH:4][N:3]=[C:2]([Cl:1])[N:7]=2)[CH:19]=[N:18][CH:17]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 775312,4-DichloropyrimidineHCID 961251H-Imidazole, 4-bromo-

生成物 1

HCID 575925314-(5-Bromo-imidazol-1-yl)-2-chloro-pyrimidine収率 23.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of 2,4-dichloropyrimidine (0.447 g, 3 mmol) in anhydrous DMF (4 ml) was added potassium carbonate (0.415 g, 3 mmol). The reaction mixture was cooled (0° C.) under an inert atmosphere before the addition of 5-bromo-1-H-imidazole (0.441 g, 3 mmol) as solution in DMF (2 ml). The reaction was then allowed to stir at this temperature for a further 3 hours whereupon water (3 ml) was added. The resultant white precipitate was removed from the mixture by filtration and washed with water before being dried to give the title compound as a white solid (0.18 g, 23%) which was suitably pure to be used without further purification. m/z (LC-MSW, ESP):259.2,261.2 (bromine isotopes) [M+H]+, R/T=3.47 mins.

後処理

  1. additionwas added
  2. customThe resultant white precipitate was removed from the mixture by filtration
  3. washwashed with water
  4. custombefore being dried

出典と根拠

ORDレコード
ord-0c6491ea44794e49912abacafa2be741
出典データセット
uspto-grants-2009_03
特許番号
US07504397B2

反応ノート

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