Methyl Isobutyl Ketone → N-METHYL-4-PHENYL-4-PIPERIDINAMINE
Reaction equation
[OH-].[K+].CC(C)CC(=O)C.C(O)(=O)C(O)=O.C(O)(=O)C(O)=O.[CH3:22][NH:23][C:24]1([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1>O>[CH3:22][NH:23][C:24]1([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:25][CH2:26][NH:27][CH2:28][CH2:29]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
6.3 g of potassium hydroxide and 15 ml of 4-methyl-2-pentanone are added at 20° C. to a solution of 7.5 g of 4-methylamino-4-phenylpiperidine dioxalate in 30 ml of water. The mixture is stirred, the phases are separated by settling and the aqueous phase is discarded. The organic phase is concentrated to dryness and the oily residue is taken up in 15 ml of toluene. The toluene solution is dried over magnesium sulfate. The minerals are filtered off and the precipitate is rinsed with 5 ml of toluene and concentrated to dryness. 3.8 g of a colorless oil, which is 4-methylamino-4-phenylpiperidine base, are thus obtained in a purity of greater than 97%.
Workup
- customthe phases are separated
- concentrationThe organic phase is concentrated to dryness
- dry with materialThe toluene solution is dried over magnesium sulfate
- filtrationThe minerals are filtered off
- washthe precipitate is rinsed with 5 ml of toluene
- concentrationconcentrated to dryness
- customare thus obtained in a purity of greater than 97%
Sources & evidence
- ORD record
- ord-753a1fecf4254913b9c39b17dabe29c9
- Source dataset
- uspto-grants-2005_07
- Patent number
- US06916929B2
Reaction notes
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