Potassium Carbonate → 2-(4-[4-(4,5-Dichloro-2-methylimidazol-1-yl)butyl]piperazin-1-yl}-5-fluoropyrimidine

HRID 1699437노트

반응식

HRID 1699437 반응식
[F:1][C:2]1[CH:3]=[N:4][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[N:6][CH:7]=1.Cl[CH2:15][CH2:16][CH2:17][CH2:18][N:19]1[C:23]([Cl:24])=[C:22]([Cl:25])[N:21]=[C:20]1[CH3:26].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:25][C:22]1[N:21]=[C:20]([CH3:26])[N:19]([CH2:18][CH2:17][CH2:16][CH2:15][N:11]2[CH2:10][CH2:9][N:8]([C:5]3[N:6]=[CH:7][C:2]([F:1])=[CH:3][N:4]=3)[CH2:13][CH2:12]2)[C:23]=1[Cl:24]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 100581585-Fluoro-2-(piperazin-1-yl)pyrimidineHCID 183205531-(4-chlorobutyl)-4,5-dichloro-2-methyl-1H-imidazole

생성물 1

HCID 98083422-(4-[4-(4,5-Dichloro-2-methylimidazol-1-yl)butyl]piperazin-1-yl}-5-fluoropyrimidine수율 83%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 3.5 g (0.02 mol) of 5-fluoro-2-(piperazin-1-yl)pyrimidine, 6.04 g (0.025 mol) of 1-(4-chlorobutyl)-4,5-dichloro-2-methyl-1H-imidazole and 4.14 g (0.03 mol) of potassium carbonate in 200 ml of dimethylformamide is maintained at reflux for 12 hours. The mixture is subsequently evaporated to dryness and the resulting crude product is redissolved in chloroform and washed repeatedly with water. The organic phase is dried and evaporated, and then the resulting crude product is purified by chromatography on a columm of silica gel. 6.4 g (83% yield) of 2-{4-[4-(4,5-dichloro-2-methylimidazol-1-yl)butyl]piperazin-1-yl}-5-fluoropyrimidine are obtained in the form of an oil.

후처리

  1. temperatureis maintained
  2. temperatureat reflux for 12 hours
  3. customThe mixture is subsequently evaporated to dryness
  4. dissolutionthe resulting crude product is redissolved in chloroform
  5. washwashed repeatedly with water
  6. customThe organic phase is dried
  7. customevaporated
  8. customthe resulting crude product is purified by chromatography on a columm of silica gel

출처 및 근거

ORD 기록
ord-a0d8b790fab84f468c5660216a655c65
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06346620B1

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