Reaction equation
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[C:7]([OH:9])=[O:8].[CH2:10]=O>C(O)=O>[CH3:10][N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[C:7]([OH:9])=[O:8]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Into a 25 ml 3-necked round bottom flask, was placed piperidine-2-carboxylic acid (975 mg, 7.56 mmol), HCHO (2.0 ml) and HCOOH (2.6 ml). The resulting solution was allowed to react, with stirring, for 5 hours while the temperature was maintained at reflux. The reaction progress was monitored by LCMS. The mixture was then concentrated by evaporation under vacuum using a rotary evaporator. The residue was triturated with 30 ml of Et2O to provide 1-methylpiperidine-2-carboxylic acid of as a white solid (0.5 g, 41%).
Workup
- customInto a 25 ml 3-necked round bottom flask, was placed
- customto react
- temperaturewas maintained
- temperatureat reflux
- concentrationThe mixture was then concentrated by evaporation under vacuum
- customa rotary evaporator
- customThe residue was triturated with 30 ml of Et2O
Sources & evidence
- ORD record
- ord-9fe4d9224b454ca3abf2f191ce757a97
- Source dataset
- uspto-grants-2014_01
- Patent number
- US08623871B2
Linked notes
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