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Chloride → 2-[3,5-Bis(trifluoromethyl)phenyl]-n{6-fluoro-6'-[(7s,9as)-7-(hydroxymethyl)hexahydropyrazino[2,1-c][1,4]oxazin-8(1h)-yl]-2-methyl-3,4'-bipyridin-3'-yl}-n,2-dimethylpropanamide

HRID 2074915
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HRID 2074915 반응식
[F:1][C:2]([F:36])([F:35])[C:3]1[CH:4]=[C:5]([C:13]([CH3:34])([CH3:33])[C:14]([N:16]([C:18]2[CH:19]=[N:20][C:21](Cl)=[CH:22][C:23]=2[C:24]2[C:25]([CH3:31])=[N:26][C:27]([F:30])=[CH:28][CH:29]=2)[CH3:17])=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.CC([Si](C)(C)[O:42][CH2:43][C@@H:44]1[CH2:53][N:52]2[C@H:47]([CH2:48][O:49][CH2:50][CH2:51]2)[CH2:46][NH:45]1)(C)C.[Cl-].[OH-].[Na+]>C1(C)C=CC=CC=1>[F:1][C:2]([F:36])([F:35])[C:3]1[CH:4]=[C:5]([C:13]([CH3:34])([CH3:33])[C:14]([N:16]([C:18]2[CH:19]=[N:20][C:21]([N:45]3[C@H:44]([CH2:43][OH:42])[CH2:53][N:52]4[C@H:47]([CH2:48][O:49][CH2:50][CH2:51]4)[CH2:46]3)=[CH:22][C:23]=2[C:24]2[C:25]([CH3:31])=[N:26][C:27]([F:30])=[CH:28][CH:29]=2)[CH3:17])=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1
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HCID 312ChlorideHCID 14798Sodium HydroxideHCID 59215768(7S,9AS)-7-(((tert-butyldimethylsilyl)oxy)methyl)octahydropyrazino[2,1-c][1,4]oxazineHCID 592158222-[3,5-bis(trifluoromethyl)phenyl]-N-(6'-chloro-6-fluoro-2-methyl-3,4'-bipyridin-3'-yl)-N,2-dimethylpropanamide

생성물 1

HCID 16063911
2-[3,5-Bis(trifluoromethyl)phenyl]-n{6-fluoro-6'-[(7s,9as)-7-(hydroxymethyl)hexahydropyrazino[2,1-c][1,4]oxazin-8(1h)-yl]-2-methyl-3,4'-bipyridin-3'-yl}-n,2-dimethylpropanamide
수율 16.4%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
90 °C

실험 절차

2-[3,5-bis(trifluoromethyl)phenyl]-N-(6′-chloro-6-fluoro-2-methyl-3,4′-bipyridin-3′-yl)-N,2-dimethylpropanamide (D54, 53.5 mg, 0.1 mmol), (7S,9aS)-7-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)octahydropyrazino[2,1-c][1,4]oxazine (D51, 37 mg, 0.13 mmol) were dissolved in toluene (1.5 mL). Bis tritertbutylphosphine palladium (13 mg, 0.026 mmol), followed by hexadecyltrimethylammoium chloride (10 μL, 25% aq sol), and finally sodium hydroxide solution (0.13 mL, 50% aq sol). The mixture was degassed for 5 minutes before heating at 90° C. for 4.5 hours. Cooled to R.T., diluted with EtOAc, washed with sat. NaHCO3 solution, dried (MgSO4). Filtered. Solvent evaporated. Residue purified by SCX column, washing with MeOH before eluting with NH3 in MeOH. Solvent evaporated. Residue purified by column chromatography eluting with Pent to EtOAc to 10% MeOH/EtOAc. Solvent evaporated under reduced pressure to afford a colourless solid of the title compound (11 mg).

후처리

  1. customThe mixture was degassed for 5 minutes
  2. temperatureCooled to R.T.
  3. additiondiluted with EtOAc
  4. washwashed with sat. NaHCO3 solution
  5. dry with materialdried (MgSO4)
  6. filtrationFiltered
  7. customSolvent evaporated
  8. customResidue purified by SCX column
  9. washwashing with MeOH
  10. washbefore eluting with NH3 in MeOH
  11. customSolvent evaporated
  12. customResidue purified by column chromatography
  13. washeluting with Pent to EtOAc to 10% MeOH/EtOAc
  14. customSolvent evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-a42c4941d57b4069b525e5f587194c6f
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919491B2

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