HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → (e)-3-(4-{[(1-Acetylpiperidin-4-yl)methylamino]methyl}phenyl)-n-(4'-chlorobiphenyl-4-yl)acrylamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Trifluoroacetic acid acetate | HCID 23437676 | — |
| Reactant | (E)-N-(4'-chlorobiphenyl-4-yl)-3-{4[(methylpiperidin-4-ylamino)methyl]phenyl}acrylamide | HCID 57845660 | — |
| Product | (e)-3-(4-{[(1-Acetylpiperidin-4-yl)methylamino]methyl}phenyl)-n-(4'-chlorobiphenyl-4-yl)acrylamide | HCID 68817916 | — |
Reaction Steps
0.017 mL (0.18 mmol) of acetic anhydride is added to a solution of 50 mg (0.087 mmol) of (E)—N-(4′-chlorobiphenyl-4-yl)-3-{4[(methylpiperidin-4-ylamino)methyl]phenyl}acrylamide×trifluoroacetic acid acetate in 4 mL of acetic acid and the mixture is stirred for 18 hours at ambient temperature. Then the reaction mixture is poured onto water and made basic with ammonia. The precipitate formed is suction filtered and washed with water. The product is dried at 60° C. in the circulating air dryer. Yield: 20 mg (46% of theory); C30H32ClN3O2 (M=502.05); melting point: 225° C.-226° C.; calc.: molecular ion peak (M+H)+: 502/504 (Cl); found: molecular ion peak (M+H)+: 502/504 (Cl).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592373B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-694b3f36366040bdbd96936d47972cdd |
| Source note | uspto-grants-2009_09 |