Ethanol → N-{3-Cyano-4-[4-(2-cyano-3-hydroxycrotonoyl)piperazin-1-yl]phenyl}-1-(4-fluorophenyl)-5-methylpyrazole-4-carboxamide

HRID 1744594노트

반응식

HRID 1744594 반응식
C(O)C.[C:4]([C:6]1[CH:7]=[C:8]([NH:26][C:27]([C:29]2[CH:30]=[N:31][N:32]([C:35]3[CH:40]=[CH:39][C:38]([F:41])=[CH:37][CH:36]=3)[C:33]=2[CH3:34])=[O:28])[CH:9]=[CH:10][C:11]=1[N:12]1[CH2:17][CH2:16][N:15]([C:18]([C:20]2[CH:21]=[N:22][O:23][C:24]=2[CH3:25])=[O:19])[CH2:14][CH2:13]1)#[N:5].[OH-].[Na+]>O>[C:4]([C:6]1[CH:7]=[C:8]([NH:26][C:27]([C:29]2[CH:30]=[N:31][N:32]([C:35]3[CH:40]=[CH:39][C:38]([F:41])=[CH:37][CH:36]=3)[C:33]=2[CH3:34])=[O:28])[CH:9]=[CH:10][C:11]=1[N:12]1[CH2:17][CH2:16][N:15]([C:18](=[O:19])/[C:20](/[C:21]#[N:22])=[C:24](\[OH:23])/[CH3:25])[CH2:14][CH2:13]1)#[N:5]

참가 물질

5

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 22228167N-{3-Cyano-4-[4-(5-methylisoxazol-4-ylcarbonyl)piperazin-1-yl]phenyl}-1-(4-fluorophenyl)-5-methylpyrazole-4-carboxamide

생성물 1

HCID 69648879N-{3-Cyano-4-[4-(2-cyano-3-hydroxycrotonoyl)piperazin-1-yl]phenyl}-1-(4-fluorophenyl)-5-methylpyrazole-4-carboxamide수율 47.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixed solvent of ethanol (10 ml) and water (10 ml) containing N-{3-cyano-4-[4-(5-methylisoxazol-4-ylcarbonyl) piperazin-1-yl]phenyl}-1-(4-fluorophenyl)-5-methylpyrazole-4-carboxamide (0.95 g) and sodium hydroxide (0.1 g) was stirred at a refluxing temperature for 2 h. The solvent was evaporated under reduced pressure. Dilute hydrochloric acid was added to the residue to allow crystallization. The crystals were recrystallized from hydrous dimethylformamide to give the title compound (0.45 g), melting point: 210° C.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. additionDilute hydrochloric acid was added to the residue
  3. customcrystallization
  4. customThe crystals were recrystallized from hydrous dimethylformamide

출처 및 근거

ORD 기록
ord-568dee4af188439a97b694b930c080b6
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07015218B1

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