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Triacetoxyperiodinane → 1,1-Dimethylethyl 4-Ethenyl-4-(phenylmethoxymethyl)-1-piperidinecarboxylate

HRID 2213030
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2213030
[CH3:1]C(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C1=CC=CC=2)=O.O[CH2:24][C:25]1([CH2:38][O:39][CH2:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:27][CH2:26]1.S(=O)(O)[O-].[Na+].C(=O)([O-])O.[Na+]>ClCCl>[CH:24]([C:25]1([CH2:38][O:39][CH2:40][C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:36])([CH3:35])[CH3:37])=[O:32])[CH2:27][CH2:26]1)=[CH2:1]
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Komponenten

6

Edukt 4

HCID 159087TriacetoxyperiodinaneHCID 516892Sodium BicarbonateHCID 219551981-Boc-4-(hydroxymethyl)-4-[(benzyloxy)methyl]piperidineHCID 23665763Sodium Bisulfite

Produkt 1

HCID 219553091,1-Dimethylethyl 4-Ethenyl-4-(phenylmethoxymethyl)-1-piperidinecarboxylateAusbeute 101,6 %

Reagenzien, Katalysatoren, Lösungsmittel

1
HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

1,1,1-Tris(acetyloxy)-1,1-dihydro-1,2-benziodoxol-3(1H)-one (1.38 g, 3.3 mmol) was added to a solution of 1,1-dimethylethyl 4-(hydroxymethyl)-4-(phenylmethoxymethyl)-1-piperidinecarboxylate (Description 95, 1.06 g, 3 mmol) in dichloromethane (40 mL) and the mixture was stirred at room temperature for 4 hours. Aqueous sodium bisulfite (10%, 10 mL) was added and the mixture was stirred at room temperature for 5 minutes. Saturated aqueous sodium hydrogen carbonate (20 mL) was added and the layers were separated. The organic layer was dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was dissolved in tetrahydrofuran (20 mL), and added to a stirred, cooled (0° C.) solution of triphenylphosphoranylidine (0.1M, 50 mL). The mixture was stirred at room temperature for 16 hours, then the solvent was evaporated under reduced pressure. Ethyl acetate (40 mL) and aqueous sodium hydrogen carbonate (10%, 40 mL) were added and the layers were separated. The organic layer was dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with isohexane/EtOAc (75:25) give the title compound (1.01 g, 99%). m/z (ES+) 332 (M+1).

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature for 5 minutes
  2. customthe layers were separated
  3. dry with materialThe organic layer was dried (MgSO4)
  4. customthe solvent was evaporated under reduced pressure
  5. dissolutionThe residue was dissolved in tetrahydrofuran (20 mL)
  6. additionadded to a stirred
  7. temperaturecooled (0° C.) solution of triphenylphosphoranylidine (0.1M, 50 mL)
  8. stirringThe mixture was stirred at room temperature for 16 hours
  9. customthe solvent was evaporated under reduced pressure
  10. additionEthyl acetate (40 mL) and aqueous sodium hydrogen carbonate (10%, 40 mL) were added
  11. customthe layers were separated
  12. dry with materialThe organic layer was dried (MgSO4)
  13. customthe solvent was evaporated under reduced pressure
  14. customThe residue was purified by flash column chromatography on silica gel
  15. washeluting with isohexane/EtOAc (75:25)

Quellen und Nachweise

ORD-Eintrag
ord-faf33270296f4658b32b656d9e75887d
Quelldatensatz
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07105507B2

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