Hydrochloric Acid → HCID 57470865, compound

HRID 2265697Notes

Reaction equation

HRID 2265697 reaction equation
[N:1]1([CH:5]2[CH2:8][N:7](C(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:6]2)[CH2:4][CH2:3][CH2:2]1.[ClH:22]>C(OCC)(=O)C>[ClH:22].[ClH:22].[N:1]1([CH:5]2[CH2:8][NH:7][CH2:6]2)[CH2:4][CH2:3][CH2:2]1

Participants

4

Procedure

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

Workup

  1. concentrationfollowed by concentration
  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. additionHexane was added to the residue
  7. customThe residue after removing a supernatant by a pipette
  8. concentrationwas concentrated under reduced pressure

Sources & evidence

ORD record
ord-d9b625cbcb684918a3cfcc6bd2262d3a
Source dataset
uspto-grants-2010_12
Patent number
US07855290B2

Reaction notes

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