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

HRID 1784384노트

반응식

HRID 1784384 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
0 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0c6491ea44794e49912abacafa2be741
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07504397B2

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