HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → N-{3-[1-(3-amino propyl)4-piperidinyl]phenyl}acetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Tert-butyl 3-{4-[3-(acetylamino)phenyl]-1-piperidinyl}propylcarbamate | HCID 22049023 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-{3-[1-(3-amino propyl)4-piperidinyl]phenyl}acetamide | HCID 21957249 | 48.1% |
Reaction Steps
TFA (1.0 mL) was added to a solution of tert-butyl N-(3-{4-[3-(acetylamino)phenyl]piperidino}propyl)carbamate (340 mg) in dry dichloromethane (10 mL) and stirred at room temperature for 5 h. A 10% aqueous solution of KOH was added to the reaction mixture until pH>6 and then the dichloromethane was removed in vacuo. The aqueous layer was frozen and lyophilized to give a solid, which was extracted with methanol. Removal of the solvent gave the desired product (120 mg) as an oil: 1H NMR (CDCl3) δ 7.23–7.16 (apparent t, 1H, J=7.5 Hz), 6.95–6.92 (m, 1H), 3.03–2.99 (m, 2H), 2.77–2.73 (t, 2H, J=6.6 Hz), 2.50–1.60 (m, 10H), 2.13 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07067534B1 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-dfb79b87db2a4d80b118626fcaea9a3e |
| Source note | uspto-grants-2006_06 |