Hydrogen Bromide → 4-(1-Methylpiperidin-3-yl)benzene-1,2-diol--hydrogen bromide (1/1)
Reaction equation
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]1Participants
3
Procedure
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.
Workup
- temperaturewas refluxed for an hour
- distillationdistilled to dryness under reduced pressure
- dissolutionThe residue was dissolved in hot ethanol
- temperaturethe solution was cooled
- filtrationvacuum filtered
Sources & evidence
- ORD record
- ord-e632f6c0e96542b191cc20acfbc3317c
- Source dataset
- uspto-grants-1978_02
- Patent number
- US04072685
Reaction notes
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