HCID 22712051, compound → HCID 22712049, compound

HRID 2121284Notes

Reaction equation

HRID 2121284 reaction equation
[ClH:1].Cl.C([N:10]1[CH2:15][CH2:14][CH:13]([N:16]([CH2:18][CH2:19][CH2:20][OH:21])[CH3:17])[CH2:12][CH2:11]1)C1C=CC=CC=1.[H][H]>CO.[Pd]>[ClH:1].[ClH:1].[OH:21][CH2:20][CH2:19][CH2:18][N:16]([CH3:17])[CH:13]1[CH2:14][CH2:15][NH:10][CH2:11][CH2:12]1

Participants

5

Reactant 2

HCID 22712051HCID 22712051, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 22712049HCID 22712049, compoundYield 183.4%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

42.8 g of 1-benzyl-4-[(3-hydroxypropyl)-methylamino]-piperidine-dihydrochloride are dissolved in 450 ml of methanol, combined with 5 g of 5% palladium-charcoal and hydrogenated at about 50° C. with hydrogen at 4-5 bar. The catalyst is filtered off, the methanol is distilled off and the residue is stirred in acetone. Ether is added, the mixture is left to stand for about two hours and then the crystals are suction filtered. 28.7 g of 4-[-(3-hydroxypropyl)-methylamino]-piperidine-dihydrochloride are obtained in the form of a solid.

Workup

  1. filtrationThe catalyst is filtered off
  2. distillationthe methanol is distilled off
  3. additionEther is added
  4. waitthe mixture is left
  5. filtrationfiltered

Sources & evidence

ORD record
ord-d49c93ac218043e1adb0862cecb872db
Source dataset
uspto-grants-2004_02
Patent number
US06696042B2

Reaction notes

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