Reaktionsgleichung
[N:1]1([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:21]=[CH:20][C:14]([C:15]([O:17]CC)=[O:16])=[CH:13][CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[ClH:22]>>[ClH:22].[N:1]1([CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:12]=[CH:13][C:14]([C:15]([OH:17])=[O:16])=[CH:20][CH:21]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1Komponenten
3
Versuchsvorschrift
A solution of ethyl 4-(3-piperidin-1-ylpropoxy)benzoate (D1) (82.57 g) in concentrated hydrochloric acid (750 ml) was heated under reflux for 2 h. The mixture was cooled to rt then chilled to 5° C. and filtered. The filter cake was washed with acetone and dried to yield the title compound (D2) as a white crystalline solid (75.30 g) that displayed MS and 1H NMR spectra that were identical to those of the product obtained by D2 (Method A).
Aufarbeitung
- temperatureunder reflux for 2 h
- temperaturethen chilled to 5° C.
- filtrationfiltered
- washThe filter cake was washed with acetone
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-fee1f30b78e144288854b0842b1d65b0
- Quelldatensatz
- uspto-grants-2008_11
- Patentnummer
- US07446103B2
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