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Hydrochloric Acid → 4-(1,3-Benzodioxol-5-yl)piperidin-4-ol

HRID 1576665
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1576665
C([N:8]1[CH2:13][CH2:12][C:11]([OH:23])([C:14]2[CH:19]=[CH:18][C:17]3[O:20][CH2:21][O:22][C:16]=3[CH:15]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1.Cl>[Pd].CO>[OH:23][C:11]1([C:14]2[CH:19]=[CH:18][C:17]3[O:20][CH2:21][O:22][C:16]=3[CH:15]=2)[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 221280344-(2H-1,3-Benzodioxol-5-yl)-1-benzylpiperidin-4-ol

Produkt 1

HCID 150347154-(1,3-Benzodioxol-5-yl)piperidin-4-ol

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

39.4 g. 1-benzyl-4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine are dissolved in 400 ml. methanol and the solution is mixed with 30 ml. 4-N hydrochloric acid. To this mixture is then added 3 g. of a palladium/carbon catalyst which has been suspended in 60 ml. alcohol. The mixture is hydrogenized at 35° - 40°C under normal pressure. After 3300 ml. hydrogen has been absorbed, hydrogenation is stopped and the cataylst is removed from the mixture by filtering. The mother liquor is heavily concentrated and the 4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine hydrochloride with a melting point of 198° - 200°C crystallizes out.

Aufarbeitung

  1. additionTo this mixture is then added 3 g
  2. customis hydrogenized at 35° - 40°C under normal pressure
  3. customhydrogen has been absorbed
  4. customthe cataylst is removed from the mixture
  5. filtrationby filtering
  6. concentrationThe mother liquor is heavily concentrated
  7. customthe 4-hydroxy-4-(3.4-methylene dioxy phenyl)-piperidine hydrochloride with a melting point of 198° - 200°C crystallizes out

Quellen und Nachweise

ORD-Eintrag
ord-89166f60b9bf43cc8968d0cdaad1fb37
Quelldatensatz
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03982001

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