Hydrochloric Acid → HCID 57470865, compound

HRID 1712643Notes

Reaction equation

HRID 1712643 reaction equation
[ClH:1].[N:2]1([CH:6]2[CH2:9][N:8](C(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:7]2)[CH2:5][CH2:4][CH2:3]1>C(OCC)(=O)C>[ClH:1].[ClH:1].[N:2]1([CH:6]2[CH2:9][NH:8][CH2:7]2)[CH2:5][CH2:4][CH2:3]1

Participants

4

Procedure

4N hydrochloric acid in ethyl acetate (1.16 ml) was added to a solution of 3-(azetidin-1-yl)-1-benzhydrylazetidine (643 mg) in ethyl acetate, and the mixture was concentrated. The resultant residue was dissolved in methanol (65 ml), and 20% palladium hydroxide (811 mg) was added thereto. This mixture was stirred under a pressurized hydrogen atmosphere (0.3 to 0.4 MPa) at room temperature for 4 hours. The catalyst was removed by filtration, and the filtrate was concentrated. The solid was suspended by the addition of heptane to the residue. The supernatant was removed using a pipette and the residue was concentrated under reduced pressure to give a crude product of the title compound (471.2 mg) as a pale yellow oil.

Workup

  1. concentrationthe mixture was concentrated
  2. dissolutionThe resultant residue was dissolved in methanol (65 ml)
  3. addition20% palladium hydroxide (811 mg) was added
  4. customThe catalyst was removed by filtration
  5. concentrationthe filtrate was concentrated
  6. additionThe solid was suspended by the addition of heptane to the residue
  7. customThe supernatant was removed
  8. concentrationthe residue was concentrated under reduced pressure

Sources & evidence

ORD record
ord-8951d81388534940ad54b42d09ff1317
Source dataset
uspto-grants-2010_09
Patent number
US07790885B2

Reaction notes

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