Hydrochloric Acid → 1-[3-(4-Chloro-phenoxy)-benzyl]-piperazine hydrochloride

HRID 331118

Reaktionsgleichung

Reaktionsgleichung von HRID 331118
C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:22]3[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=3)[CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.O.Cl.C1COCC1>O1CCOCC1>[ClH:28].[Cl:28][C:25]1[CH:26]=[CH:27][C:22]([O:21][C:17]2[CH:16]=[C:15]([CH:20]=[CH:19][CH:18]=2)[CH2:14][N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[CH:23][CH:24]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8028TetrahydrofuranHCID 674135414-[3-(4-Chloro-phenoxy)-benzyl]-piperazine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 674138091-[3-(4-Chloro-phenoxy)-benzyl]-piperazine hydrochlorideAusbeute 211,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

A solution of 4-[3-(4-chloro-phenoxy)-benzyl]-piperazine-1-carboxylic acid tert-butyl ester (29.6 g, 73.5 mmol) in 4:1 dioxane:H2O (100 mL) was treated with 4 M HCl in dioxane (60 mL). After 3 h, THF (200 mL) was added and the resulting white precipitate was filtered and dried under vacuum to give 1-[3-(4-chloro-phenoxy)-benzyl]-piperazine hydrochloride (26.4 g, 95%). MS (ESI+): calcd for C17H19ClN2O m/z 302.12, found 303.1 (M+H)+.

Aufarbeitung

  1. filtrationthe resulting white precipitate was filtered
  2. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f795602b1ab64b009dcf27a6892b050c
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08877769B2

Verknüpfte Notizen

Wird geladen…