Hydrogen Bromide → HCID 66703158, compound

33% hydrogen bromide in glacial acetic acid (20 ml) was added to a solution of benzyl 4-((dimethylamino)(phenyl)methyl)piperidine-1-carboxylate (2.32 g, 6.58 mmol) in glacial acetic acid (20 ml), and stirring was carried out for 1.5 h at room temperature. A solid was precipitated by addition of diethyl ether. The supernatant solution was decanted off; diethyl ether was added repeatedly to the residue, and the supernatant solution was decanted off again each time. The residue was dried in vacuo and dissolved in methanol (20 ml); strongly basic ion exchanger Dowex 1×2-200 was added thereto, and stirring was carried out for 1 h at room temperature. The mixture was then filtered, the filter residue was washed with methanol, and the filtrate was concentrated in vacuo.

1. customA solid was precipitated by addition of diethyl ether
2. customThe supernatant solution was decanted off
3. additiondiethyl ether was added repeatedly to the residue
4. customthe supernatant solution was decanted off again each time
5. customThe residue was dried in vacuo
6. dissolutiondissolved in methanol (20 ml)
7. additionstrongly basic ion exchanger Dowex 1×2-200 was added
8. stirringstirring
9. waitwas carried out for 1 h at room temperature
10. filtrationThe mixture was then filtered
11. washthe filter residue was washed with methanol
12. concentrationthe filtrate was concentrated in vacuo

ORD record

ord-c40aa0b44bd94138bb0bcfbc5b1a8e70

Source dataset

uspto-grants-2012_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08119633B2