Methyl Isobutyl Ketone → N-METHYL-4-PHENYL-4-PIPERIDINAMINE

HRID 895793Notes

Reaction equation

HRID 895793 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]1

Participants

5

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

  1. customthe phases are separated
  2. concentrationThe organic phase is concentrated to dryness
  3. dry with materialThe toluene solution is dried over magnesium sulfate
  4. filtrationThe minerals are filtered off
  5. washthe precipitate is rinsed with 5 ml of toluene
  6. concentrationconcentrated to dryness
  7. 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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