Hydrochloric Acid → 1,4-Dimethylpiperazine-2-carboxylic acid
Reaction equation
C([O:3][C:4]([CH:6]1[CH2:11][N:10]([CH3:12])[CH2:9][CH2:8][N:7]1[CH3:13])=[O:5])C.[OH-].[Na+].Cl.CCOCC>CCO>[CH3:13][N:7]1[CH2:8][CH2:9][N:10]([CH3:12])[CH2:11][CH:6]1[C:4]([OH:5])=[O:3]Participants
6
Procedure
Ethyl 1,4-dimethylpiperazin-2-yl carboxylic acid (1.86 g) was dissolved in EtOH (10 mL) and 5M aqueous NaOH (20 mL) added. The mixture was refluxed for 2 hours, allowed to cool, 10M HCl (9.1 mL) added to give pH4 and the mixture evaporated to dryness. The white solid was stirred with MeOH (25 mL), CH2Cl2 (10 mL) added and the filtrate evaporated to give, after trituration with Et2O, the title compound as a grey solid (761 mg, 48%).
Workup
- temperatureThe mixture was refluxed for 2 hours
- temperatureto cool
- customto give pH4
- customthe mixture evaporated to dryness
- additionadded
- customthe filtrate evaporated
- customto give
Sources & evidence
- ORD record
- ord-fe32eb0156d34e94a22331c6aa679761
- Source dataset
- uspto-grants-2011_03
- Patent number
- US07906645B2
Reaction notes
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