Hydrogen Bromide → 4-(1-Methylpiperidin-3-yl)benzene-1,2-diol--hydrogen bromide (1/1)
Reaktionsgleichung
Cl.[CH3:2][N:3]1[CH2:8][CH2:7][CH2:6][CH:5]([C:9]2[CH:14]=[CH:13][C:12]([O:15]C)=[C:11]([O:17]C)[CH:10]=2)[CH2:4]1.[BrH:19]>>[BrH:19].[CH3:2][N:3]1[CH2:8][CH2:7][CH2:6][CH:5]([C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[C:11]([OH:17])[CH:10]=2)[CH2:4]1Komponenten
3
Versuchsvorschrift
A mixture of 8 g of the product of Step D in 40 ml of 66% hydrobromic acid was refluxed for an hour and then distilled to dryness under reduced pressure. The residue was dissolved in hot ethanol and the solution was cooled and vacuum filtered to obtain 2.49 g of N-methyl-3-(3',4'-dihydroxyphenyl)-piperidine hydrobromide as crystals melting at 190° C.
Aufarbeitung
- temperaturewas refluxed for an hour
- distillationdistilled to dryness under reduced pressure
- dissolutionThe residue was dissolved in hot ethanol