Hydrochloric Acid → HCID 15023840, compound

A mixture of a suspension of 5.03 g (0.015 mole) of 1,4-dibenzyl-2,6-bis(fluoromethyl)piperazine isomer B [prepared as described in step (b) above] in 130 ml of methanol and 6 ml of concentrated aqueous hydrochloric acid was stirred vigorously under a stream of hydrogen at room temperature for 1 hour in the presence of 0.6 g of 20% w/w palladium-on-carbon. At the end of this time, the catalyst was removed by filtration, and the filtrate was concentrated by evaporation under reduced pressure. The residue was mixed with 50 ml of water, and the resulting insoluble materials were removed by filtration. The filtrate was concentrated by evaporation under reduced pressure, and the residue was washed with ethanol, to afford 3.10 g of 2,6-bis(fluoromethyl)piperazine (isomer B) dihydrochloride as a colorless powder, melting at 207°-225° C.

1. customAt the end of this time, the catalyst was removed by filtration
2. concentrationthe filtrate was concentrated by evaporation under reduced pressure
3. additionThe residue was mixed with 50 ml of water
4. customthe resulting insoluble materials were removed by filtration
5. concentrationThe filtrate was concentrated by evaporation under reduced pressure
6. washthe residue was washed with ethanol

ORD record

ord-268767e2fd5e47ef91a2d3405222629a

Source dataset

uspto-grants-1996_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05496951