Hydrogen Bromide → HCID 21473473, compound
Reaction equation
Cl.[CH3:2][O:3][C:4]1[CH:9]=[C:8]([O:10]C)[CH:7]=[CH:6][C:5]=1[N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.[BrH:18]>>[BrH:18].[BrH:18].[OH:10][C:8]1[CH:7]=[CH:6][C:5]([N:12]2[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]2)=[C:4]([O:3][CH3:2])[CH:9]=1Participants
3
Procedure
A mixture of 1-(2,4-dimethoxyphenyl) piperazine hydrochloride (3.1 g, 13.9 mmol) in 30 mL of approximately 40% aqueous hydrogen bromide was heated at reflux for 30 hours and then the volatiles were removed in vacuo. Recrystallization of the residue from methanol gave 1-(4-hydroxy-2-methoxyphenyl)piperazine dihydrobromide (4.6 g, 12.4 mmol), m.p. >280° C.
Workup
- temperaturewas heated
- temperatureat reflux for 30 hours
- customthe volatiles were removed in vacuo
- customRecrystallization of the residue from methanol
Sources & evidence
- ORD record
- ord-37c853c6a8ed40e9a598f3d0232413f7
- Source dataset
- uspto-grants-1997_11
- Patent number
- US05688795
Reaction notes
Loading…