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Hydrochloric Acid → 4a-Methyl-6-(phenylsulfonyl)-1,2,3,4,4a,9a-hexahydro[1]benzofuro[2,3-c]pyridine hydrochloride

HRID 1616874
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1616874
C(O[C:6]([N:8]1C[CH2:12][C:11]2(C)[C:14]3[CH:20]=[C:19]([S:21][C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[CH:18]=[CH:17][C:15]=3O[CH:10]2[CH2:9]1)=O)(C)(C)C.[CH3:29][OH:30].[OH2:31].[OH:32]OS([O-])=O.[K+].O1CCOCC1.[ClH:44]>C(OCC)(=O)C>[ClH:44].[CH3:12][C:11]12[C:14]3[CH:20]=[C:19]([S:21]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)(=[O:32])=[O:31])[CH:18]=[CH:17][C:15]=3[O:30][CH:29]1[CH2:6][NH:8][CH2:9][CH2:10]2
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Komponenten

8

Edukt 6

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962WaterHCID 312751,4-DioxaneHCID 23707502Potassium hydroxy sulfiteHCID 673240934a-Methyl-6-(phenylsulfanyl)-1,2,3,4,4a,9-hexahydro[1]benzofuro[2,3-c]pyridine-2-carboxylic acid tert-butyl ester

Produkt 1

HCID 67325154
4a-Methyl-6-(phenylsulfonyl)-1,2,3,4,4a,9a-hexahydro[1]benzofuro[2,3-c]pyridine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 4a-methyl-6-(phenylsulfanyl)-1,2,3,4,4a,9a-hexahydro[1]benzofuro[2,3-c]pyridine-2-carboxylic acid tert-butyl ester (0.327 g, 0.82 mmol) in methanol (10 mL, 0.2 mol) was added water (0.5 mL, 0.03 mol) and Oxone® (2.0 g, 0.0032 mol). The reaction was stirred overnight at room temperature. The reaction mixture was filtered and the filtrate concentrated. The residue was dissolved in DCM and washed with brine, dried, filtered and concentrated. The crude product was purified on a 12 g silica gel column eluting with hexanes to 2:1 hexanes:ethyl acetate and then stirred in 4 M HCl in dioxane (5 mL, 0.04 mol) for 30 min. The product was precipitated by addition of DCM and ether. The solid was filtered, washed with ether and dried under house vacuum to afford the title compound. mp 236-238° C. dec.; MS m/z 330 [M+H]+. 1H-NMR (400 MHz, DMSO): δ 1.45 (s, 3H), 1.75 (m, 1H), 1.90 (m, 1H), 2.82 (m, 1H), 3.03 (m, 1H), 3.35-3.56 (m, 2H), 4.63 (s, 1H), 7.08 (d, J=8.9 Hz, 1H), 7.58-7.70 (m, 3H), 7.81 (d, J=8.85 Hz, 1H), 7.91-7.96 (m, 3H), 8.91 (bs, 1H), 9.91 (bs, 1H).

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate concentrated
  3. dissolutionThe residue was dissolved in DCM
  4. washwashed with brine
  5. customdried
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude product was purified on a 12 g silica gel column
  9. washeluting with hexanes to 2:1 hexanes
  10. customThe product was precipitated by addition of DCM and ether
  11. filtrationThe solid was filtered
  12. washwashed with ether
  13. customdried under house vacuum

Quellen und Nachweise

ORD-Eintrag
ord-808b9f79a43048718126be74b1ef64b9
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08765779B2

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