1-Butanaminium, N,N,N-tributyl-, fluoride, hydrate → HCID 16222146, 화합물

HRID 1717392노트

반응식

HRID 1717392 반응식
Br[CH2:2][CH2:3][CH2:4][C:5]1[N:9]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([NH:18][CH2:19][C:20]([F:23])([F:22])[F:21])=[O:17])=[CH:12][CH:11]=2)[N:8]=[N:7][C:6]=1[C:24]([NH:26][CH:27]1[CH2:29][CH2:28]1)=[O:25].O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C(#N)C>[CH:27]1([NH:26][C:24]([C:6]2[N:7]=[N:8][N:9]([C:10]3[CH:15]=[CH:14][C:13]([C:16]([NH:18][CH2:19][C:20]([F:21])([F:22])[F:23])=[O:17])=[CH:12][CH:11]=3)[C:5]=2/[CH:4]=[CH:3]/[CH3:2])=[O:25])[CH2:29][CH2:28]1

참가 물질

4

반응물 2

HCID 162116731-Butanaminium, N,N,N-tributyl-, fluoride, hydrateHCID 68514522HCID 68514522, 화합물

생성물 1

HCID 16222146HCID 16222146, 화합물수율 16%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

5-(3-Bromopropyl)-N-cyclopropyl-1-(4-{[(2,2,2-trifluoroethyl)amino]carbonyl}phenyl)-1H-1,2,3-triazole-4-carboxamide (212 mg, 0.45 mmol) obtained in Example 399a) was dissolved in acetonitrile (5.0 ml), tetrabutylammonium fluoride monohydrate (140 mg, 0.54 mmol) was added, and the mixture was stirred at 80° C. for 16 hr. The reaction mixture was allowed to cool to room temperature and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (ethyl acetate/hexane=1/9 to 7/3) and recrystallized from ethyl acetate-hexane to give the title compound as a colorless powder (27.7 mg, 16%).

후처리

  1. temperatureto cool to room temperature
  2. customthe solvent was evaporated under reduced pressure
  3. customThe residue was purified by silica gel column (ethyl acetate/hexane=1/9 to 7/3)
  4. customrecrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-f3d877944089492ebc35e1a1f5528a93
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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