HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18770386, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1,4-Bis[(1-tert-butoxycarbonyl-4-piperidinyl)methyl]piperazine | HCID 18770426 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18770386 | HCID 18770386 | 84% |
Reaction Steps
A 4N hydrogen chloride in ethyl acetate (4 ml; 16 mmol) was added to a solution in methylene chloride (2 ml) of 1,4-bis[(1-tert-butoxycarbonyl-4-piperidinyl)methyl]-piperazine (195 mg; 0.40 mmol) synthesized by the above process under ice cooling, and the mixture was stirred for 30 minutes. The ice bath was removed, and the mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated under reduced pressure, and the resultant crude crystals were recrystallized from methylene chloride-methanol-diethyl ether, thereby obtaining 154 mg (yield: 84%) of the title compound as a colorless crystalline powder (melting point: 280° C. or higher).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06448242B1 |
| Source dataset | uspto-grants-2002_09 |
| ORD ID | ord-5ad890fbd0d0425eb7193850281ddaac |
| Source note | uspto-grants-2002_09 |