HCID 22712051, compound → HCID 22712049, compound

HRID 352430Notes

Reaction equation

HRID 352430 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]>[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

4

Reactant 2

HCID 22712051HCID 22712051, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 22712049HCID 22712049, compoundYield 183.4%

Reagents, catalysts & solvents 1

HCID 23938PalladiumCatalyst

Procedure

42.8 g of 1-benzyl-4-[(3-hydroxypropyl)-methylamino]-piperidine-dihydrochloride are dissolved in 450 ml of methaol, combined with 5 g of 5% palladium/charcoal and hydrogenated at about 50° C. with hydrogen at a pressure of 4-5 bar. The catalyst is filtered off, the methanol is distilled off and the residue is stirred into 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 as 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-12292aec1c514aacbc9c5cb359ecf087
Source dataset
uspto-grants-2004_06
Patent number
US06747044B2

Reaction notes

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