Potassium Carbonate → 4-Morpholinopiperidine

HRID 2065479Notes

Reaction equation

HRID 2065479 reaction equation
Cl.Cl.C1(C[N:10]2[CH2:15][CH2:14][CH:13]([N:16]3[CH2:21][CH2:20][O:19][CH2:18][CH2:17]3)[CH2:12][CH2:11]2)C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>C(O)(C)(C)C.O>[NH:10]1[CH2:15][CH2:14][CH:13]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)[CH2:12][CH2:11]1

Participants

5

Reactant 2

HCID 11430Potassium CarbonateHCID 67094508HCID 67094508, compound

Product 1

HCID 7957244-Morpholinopiperidine

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×HCID 6386tert-ButanolSolvent

Procedure

10.00 kg (30.00 mol) 4-[1-(phenylmethyl)-4-piperidinyl]-morpholine-dihydrochloride (M) were suspended in 50.0 L tert-butanol and 10.0 L water and heated to 45° C. At 45° C. a solution of 10.37 kg (75.01 mol) potassium carbonate in 24.0 L water was metered in. Then the aqueous phase was separated off at 45° C. and 20.0 L solvent were distilled off in vacuo. The mixture was then hydrogenated at a pressure of 4 bar and an internal temperature of 60° C. until no further uptake of hydrogen could be detected. After the reaction was complete, the catalyst was filtered off and the residue was washed with 20.0 L tert-butanol.

Workup

  1. customAt 45° C.
  2. customThen the aqueous phase was separated off at 45° C.
  3. distillation20.0 L solvent were distilled off in vacuo
  4. customan internal temperature of 60° C.
  5. filtrationthe catalyst was filtered off
  6. washthe residue was washed with 20.0 L tert-butanol

Sources & evidence

ORD record
ord-939c4cd9af6344f4b3a97b1bfc0884ac
Source dataset
uspto-grants-2012_10
Patent number
US08288531B2

Reaction notes

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