HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen chloride-ethyl acetate → 4-chloro-N-[(3R,4R)-3-(3,4-dichlorophenyl)-1-(piperidin-4-ylmethyl)piperidin-4-yl]-N-methylbenzamide Monohydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | tert-butyl 4-{[(3R,4R)-4-{[(4-chlorophenyl)carbonyl](methyl)amino}-3-(3,4-dichlorophenyl)piperidin-1-yl]methyl}piperidine-1-carboxylate | HCID 68932507 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 4-chloro-N-[(3R,4R)-3-(3,4-dichlorophenyl)-1-(piperidin-4-ylmethyl)piperidin-4-yl]-N-methylbenzamide Monohydrochloride | HCID 68930185 | 168% |
Reaction Steps
To a solution of tert-butyl 4-{[(3R,4R)-4-{[(4-chlorophenyl)carbonyl] (methyl)amino}-3-(3,4-dichlorophenyl)piperidin-1-yl]methyl}piperidine-1-carboxylate (200 mg) obtained in Example 461 in ethyl acetate (4 mL) was added 4N hydrogen chloride/ethyl acetate (4 mL), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure to give the title compound (150 mg, 85%) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08470816B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-2636478c35ec494c97a4700ed18048ca |
| Source note | uspto-grants-2013_06 |