Water → 4-(Azetidin-1-yl)piperidine dihydrochloride

HRID 492847Notes

Reaction equation

HRID 492847 reaction equation
[ClH:1].Cl.[N:3]1([CH:7]2[CH2:12][CH2:11][N:10](CC3C=CC=CC=3)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4]1.O>CC(O)C.[C].[Pd]>[ClH:1].[ClH:1].[N:3]1([CH:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4]1

Participants

5

Procedure

After adding 10% palladium-carbon (600 mg) to a solution of the crude 4-(azetidin-1-yl)-1-benzylpiperidine dihydrochloride (6.55 g) in 2-propanol (50 ml)-water (50 ml), the mixture was stirred for 23 hours at room temperature under a hydrogen atmosphere. The catalyst was filtered and washed with 2-propanol, and then the filtrate was concentrated. Ethanol (10 ml)-hexane (50 ml) was added to the residue to produce suspended precipitate. It was then filtered and washed with 10 ml of ethanol. The filtered precipitate was subjected to aeration drying to provide the title compound (4.26 g) as white powder.

Workup

  1. filtrationThe catalyst was filtered
  2. washwashed with 2-propanol
  3. concentrationthe filtrate was concentrated
  4. additionEthanol (10 ml)-hexane (50 ml) was added to the residue
  5. customto produce
  6. filtrationIt was then filtered
  7. washwashed with 10 ml of ethanol
  8. customdrying

Sources & evidence

ORD record
ord-b94a7eedcb6a491bb16c395c0a673a75
Source dataset
uspto-grants-2009_05
Patent number
US07531532B2

Reaction notes

Loading…