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Acetic Acid → rac-(2'S,3'S,4'S)-6-chloro-2'-(3-chloro-2-fluoro-phenyl)-4'-(3-hydroxy-2,2-dimethyl-propyl)-1H-spiro[indole-3,3'-pyrrolidin]-2-one

HRID 2065410
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HRID 2065410 반응식
C(OC([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([Cl:17])[CH:15]=2)/[C:10](=[CH:18]/[CH2:19][C:20]([CH3:31])([CH3:30])[CH2:21][O:22][Si](C(C)(C)C)(C)C)/[C:9]1=[O:32])=O)(C)(C)C.[Cl:33][C:34]1[C:35]([F:47])=[C:36](/[CH:40]=[N:41]/[CH2:42][Si](C)(C)C)[CH:37]=[CH:38][CH:39]=1.C(O)(=O)C.O>CN(C)P(N(C)C)(N(C)C)=O>[Cl:17][C:14]1[CH:15]=[C:16]2[NH:8][C:9](=[O:32])[C:10]3([CH:18]([CH2:19][C:20]([CH3:30])([CH3:31])[CH2:21][OH:22])[CH2:42][NH:41][CH:40]3[C:36]3[CH:37]=[CH:38][CH:39]=[C:34]([Cl:33])[C:35]=3[F:47])[C:11]2=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962Water2회HCID 58398999(E)-1-(3-chloro-2-fluorophenyl)-N-(trimethylsilylmethyl)methanimineHCID 86656669Z-3-[4-(tert-butyl-dimethyl-silanyloxy)-3,3-dimethyl-butylidene]-6-chloro-2-oxo-2,3-dihydro-indole-1-carboxylic acid tert-butyl ester

생성물 1

HCID 67338072
rac-(2'S,3'S,4'S)-6-chloro-2'-(3-chloro-2-fluoro-phenyl)-4'-(3-hydroxy-2,2-dimethyl-propyl)-1H-spiro[indole-3,3'-pyrrolidin]-2-one

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매

실험 절차

To a solution of E/Z-3-[4-(tert-butyl-dimethyl-silanyloxy)-3,3-dimethyl-butylidene]-6-chloro-2-oxo-2,3-dihydro-indole-1-carboxylic acid tert-butyl ester prepared in Example 31 (2.5 g, 5.2 mmol) in hexamethylphosphoramide (30 mL) was added [1-(3-chloro-2-fluoro-phenyl)-meth-(E)-ylidene]-trimethylsilanylmethyl-amine prepared in Example 5 (2.9 g, 12 mmol), acetic acid (0.75 g, 12 mmol) and H2O (0.25 g, 14 mmol) sequentially. The reaction mixture was stirred at room temperature for 24 h. Water was added. The mixture was extracted with ethyl acetate. The organic layer was separated, and aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with water twice, dried over MgSO4, then concentrated. The residue was dissolved into dichloromethane (10 mL), and trifluoroacetic acid (5 mL) was added. The reaction mixture was stirred at room temperature for 1 h. The mixture was concentrated, and the residue was partitioned between ethyl acetate and aqueous saturated NaHCO3 solution. The organic layer was separated, dried over MgSO4, then concentrated. The residue was dissolved into tetrahydrofuran (5 mL), and saturated aqueous NaHCO3 solution was added (5 mL). The reaction mixture was stirred at room temperature for 1 h. The mixture was concentrated, and the residue was partitioned between ethyl acetate and water. The organic layer was separated, dried over MgSO4, then concentrated. The residue was purified by chromatography (3% MeOH in EtOAc) to give rac-(2′S,3′S,4′S)-6-chloro-2′-(3-chloro-2-fluoro-phenyl)-4′-(3-hydroxy-2,2-dimethyl-propyl)-1H-spiro[indole-3,3′-pyrrolidin]-2-one as a white solid (Yield, 0.25 g, 11%).

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. customThe organic layer was separated
  3. extractionaqueous layer was extracted with ethyl acetate
  4. washwashed with water twice
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. dissolutionThe residue was dissolved into dichloromethane (10 mL), and trifluoroacetic acid (5 mL)
  8. additionwas added
  9. stirringThe reaction mixture was stirred at room temperature for 1 h
  10. concentrationThe mixture was concentrated
  11. customthe residue was partitioned between ethyl acetate and aqueous saturated NaHCO3 solution
  12. customThe organic layer was separated
  13. dry with materialdried over MgSO4
  14. concentrationconcentrated
  15. dissolutionThe residue was dissolved into tetrahydrofuran (5 mL), and saturated aqueous NaHCO3 solution
  16. additionwas added (5 mL)
  17. stirringThe reaction mixture was stirred at room temperature for 1 h
  18. concentrationThe mixture was concentrated
  19. customthe residue was partitioned between ethyl acetate and water
  20. customThe organic layer was separated
  21. dry with materialdried over MgSO4
  22. concentrationconcentrated
  23. customThe residue was purified by chromatography (3% MeOH in EtOAc)
  24. customto give

출처 및 근거

ORD 기록
ord-46216d0681284ed3a6e6710b4e741494
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288431B2

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