Hydrochloric Acid → 1-[1-(4-Pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride

HRID 2086235Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2086235
C(OC([N:11]1[CH2:16][CH2:15][N:14]([NH:17][CH:18]2[CH2:23][CH2:22][N:21]([C:24]3[CH:29]=[CH:28][N:27]=[CH:26][CH:25]=3)[CH2:20][CH2:19]2)[C:13](=[O:30])[CH2:12]1)=O)C1C=CC=CC=1.[ClH:31]>C(OCC)(=O)C.CO.[Pd]>[ClH:31].[ClH:31].[ClH:31].[N:27]1[CH:28]=[CH:29][C:24]([N:21]2[CH2:20][CH2:19][CH:18]([NH:17][N:14]3[CH2:15][CH2:16][NH:11][CH2:12][C:13]3=[O:30])[CH2:23][CH2:22]2)=[CH:25][CH:26]=1

Komponenten

6

Edukt 2

HCID 313Hydrochloric AcidHCID 178254544-Benzyloxycarbonyl-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone

Produkt 1

HCID 695456121-[1-(4-Pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of 4-benzyloxycarbonyl-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (25.29 g) and an a 4N solution of hydrochloric acid in ethyl acetate (15.5 ml) in methanol (300 ml) was combined with 10% Pd/C (50% hydrated, 5.00 g) and stirred at room temperature for 15 hours under a hydrogen atmosphere. The catalyst was filtered off, and the reaction mixture was concentrated. The residue was dissolved in ethanol (300 ml), and combined with a 4N solution of hydrochloric acid in ethyl acetate (31 ml). The crystals precipitated were collected by filtration and dried to obtain 1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride (20.16 g) as colorless crystals.

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. concentrationthe reaction mixture was concentrated
  3. dissolutionThe residue was dissolved in ethanol (300 ml)
  4. customThe crystals precipitated
  5. filtrationwere collected by filtration
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0d55b9eb262941a982003bef791d5c1f
Quelldatensatz
uspto-grants-2004_04
Patentnummer
US06723722B1

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