Acetone → 4-(4-(Propan-2-yl)piperazin-1-yl)benzoic acid hydrochloride

HRID 478629

Reaktionsgleichung

Reaktionsgleichung von HRID 478629
C[O:2][C:3](=[O:19])[C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][N:13]([CH:16]([CH3:18])[CH3:17])[CH2:12][CH2:11]2)=[CH:6][CH:5]=1.CC(C)=O.[ClH:24]>>[ClH:24].[CH:16]([N:13]1[CH2:14][CH2:15][N:10]([C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:19])=[O:2])=[CH:5][CH:6]=2)[CH2:11][CH2:12]1)([CH3:18])[CH3:17]

Komponenten

4

Reaktionsbedingungen

Temperatur
2 °C

Versuchsvorschrift

4-(4-Isopropyl-piperazin-1-yl)-benzoic acid methyl ester (0.9 mmol) is dissolved in 4N HCl (2 ml) and heated under reflux for 7 hours. The mixture is cooled in an ice bath to 0-4° C. and acetone is added. The solid material formed is filtered off, washed with cold acetone and dried (vacuum). A pale-brown powder with mp. >270° C., Rf=0.08 (CH2Cl2/MeOH=9:1) is obtained.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 7 hours
  3. customThe solid material formed
  4. filtrationis filtered off
  5. washwashed with cold acetone
  6. customdried (vacuum)
  7. customA pale-brown powder with mp. >270° C., Rf=0.08 (CH2Cl2/MeOH=9:1) is obtained

Quellen und Nachweise

ORD-Eintrag
ord-cfc40f076cc64d3a88489e8e7a488252
Quelldatensatz
uspto-grants-2003_11
Patentnummer
US06642239B2

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