HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-(Acetylthio)-1-[(E)-4-(trifluoromethoxy)cinnamoyl]-piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (E)-3-[4-(trifluoromethoxy)phenyl]prop-2-enoyl chloride | HCID 5709512 | — |
| Reactant | 4-(Acetylthio)piperidine hydrochloride | HCID 18363290 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-(Acetylthio)-1-[(E)-4-(trifluoromethoxy)cinnamoyl]-piperidine | HCID 18363273 | 95.2% |
Reaction Steps
In 17 ml of dichloromethane were suspended 1.28 g (6.53 mmol) of 4-(acetylthio)piperidine hydrochloride, and 2.27 ml (16.3 mmol) of triethylamine were added dropwise to the suspension with stirring under ice-cooling. Then, a solution in which 1.80 g (7.18 mmol) of (E)-4-(trifluoromethoxy)cinnamoyl chloride were dissolved in 6 ml of dichloromethane was added dropwise to the reaction mixture, followed by stirring of the mixture at the same temperature for 1 hour. The reaction mixture was subjected to silica gel column chromatography and eluted with a mixed solvent of hexane-ethyl acetate (2:1 to 1:1) to obtain 2.32 g (yield: 95%) of the desired compound as a slightly yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06300357B1 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-45d039b579d548aa81698df587e44efc |
| Source note | uspto-grants-2001_10 |