Hydrochloric Acid → 4-amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide

HRID 430688Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 430688
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH:15][C:16]([C:18]2[CH:23]=[C:22]([Cl:24])[C:21]([NH2:25])=[CH:20][C:19]=2[O:26][CH3:27])=[O:17])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>CO.C(OCC)C>[NH2:25][C:21]1[C:22]([Cl:24])=[CH:23][C:18]([C:16]([NH:15][CH2:14][CH:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[O:17])=[C:19]([O:26][CH3:27])[CH:20]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 11200348N-tert-butyloxycarbonyl-4-(4-amino-5-chloro-2-methoxyphenylcarbonylaminomethyl)piperidine

Produkt 1

HCID 98177134-amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of N-tert-butyloxycarbonyl-4-(4-amino-5-chloro-2-methoxyphenyl-carbonylaminomethyl)piperidine (500 mg, 1.26 mmol) in methanol solution (30 ml) was added an ethereal 1N hydrogen chloride solution (12.6 ml, 12.6 mmol). The solution was heated at 50° C. The reaction mixture became heterogeneous within 5 min. After 1.5 h, the reaction mixture was concentrated to give a white solid which was suspended in diethylether and filtered to give 4-(4-amino-5-chloro-2-methoxyphenylcarbonylaminomethyl)piperidine as a bis-hydrochloride salt (433 mg).

Aufarbeitung

  1. waitAfter 1.5 h
  2. concentrationthe reaction mixture was concentrated
  3. customto give a white solid which
  4. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-36b00c989d4d44a6ade78abea022242a
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06323223B1

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