Hydrochloric Acid → Benzphetamine Hydrochloride

HRID 1047588

Reaktionsgleichung

Reaktionsgleichung von HRID 1047588
[ClH:1].[CH3:2][C@H:3]([N:11]([CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[CH3:12])[CH2:4][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1>C(OCC)(=O)C>[CH3:2][C@H:3]([N:11]([CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:12])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[ClH:1]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 5311017Benzphetamine

Produkt 1

HCID 11558159Benzphetamine Hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Reaktionsbedingungen

Temperatur
12.5 °C

Versuchsvorschrift

Ethyl acetate (810 ml) containing 10% HCl was added to the crude benzphetamine free base isolated from Example 1 at 10-15° C. The mixture was stirred for 30 min at 10-15° C. and then stirred at 25°˜30° C. for 8-10 hours. Excess hydrochloric acid gas was removed by concentration of the solvent to give a solid. The reaction mass was cooled to 0-5° C. Ethyl acetate (1500 ml) was added to the mixture and was stirred for 1 h at 25° C. The solid obtained was filtered and was washed with ethyl acetate (1000 ml). The solid obtained was dried for 6 h under vacuum at 55° C.-60° C.

Aufarbeitung

  1. stirringstirred at 25°˜30° C. for 8-10 hours
  2. customExcess hydrochloric acid gas was removed by concentration of the solvent
  3. customto give a solid
  4. temperatureThe reaction mass was cooled to 0-5° C
  5. stirringwas stirred for 1 h at 25° C
  6. customThe solid obtained
  7. filtrationwas filtered
  8. washwas washed with ethyl acetate (1000 ml)
  9. customThe solid obtained
  10. customwas dried for 6 h under vacuum at 55° C.-60° C.

Quellen und Nachweise

ORD-Eintrag
ord-10a6e4e8ed1c4cda94fdca1a6b57006c
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08569544B2

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