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Hydrochloric Acid → 3-(4-Bromophenyl)piperidine

HRID 1784707
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1784707
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][CH2:12][CH2:11][NH:10][C:9]2=O)=[CH:4][CH:3]=1.B.O1CCCC1.Cl>O1CCCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:13][CH2:12][CH2:11][NH:10][CH2:9]2)=[CH:6][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 2723981Borane;tetrahydrofuranHCID 468400403-(4-Bromophenyl)piperidin-2-one

Produkt 1

HCID 468353263-(4-Bromophenyl)piperidineAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To an ice-cooled solution of 3-(4-bromo-phenyl)-piperidin-2-one (37.97 g, 149 mmol) in tetrahydrofuran (250 ml) was added borane-tetrahydrofuran complex (335 ml, 1.0 M solution in THF, 335 mmol). The solution was stirred overnight at room temperature, and then refluxed 1.5 hr after addition of 10% aqueous hydrochloric acid. Solvents was removed in vacuo, and the residue was partitioned between dichloromethane and 1N sodium hydroxide. The aqueous layer was extracted with dichlorometane. The combined organic layer was washed with water and brine, dried over sodium sulfate, and concentrated in vacuo. The residue was dissolved in water (100 mL) and concentrated hydrochloric acid (100 mL) and refluxed for 3 hr. Sodium hydroxide was added to the solution and the resulting solution was extracted with dichlorometane. The organic layer was washed with water and brine, dried over sodium sulfate Concentration in vacuo afforded 3-(4-bromo-phenyl)-piperidine (32 18 g, 90%).

Aufarbeitung

  1. temperaturerefluxed 1.5 hr
  2. customSolvents was removed in vacuo
  3. customthe residue was partitioned between dichloromethane and 1N sodium hydroxide
  4. extractionThe aqueous layer was extracted with dichlorometane
  5. washThe combined organic layer was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. dissolutionThe residue was dissolved in water (100 mL)
  9. temperatureconcentrated hydrochloric acid (100 mL) and refluxed for 3 hr
  10. additionSodium hydroxide was added to the solution
  11. extractionthe resulting solution was extracted with dichlorometane
  12. washThe organic layer was washed with water and brine
  13. dry with materialdried over sodium sulfate Concentration in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-6d4e95c7133d42b48eeb2ffe5e987cab
Quelldatensatz
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07504411B2

Notizen zur Reaktion

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