HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24804837, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Malonic Acid | HCID 867 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | HCID 58007713 | HCID 58007713 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 24804837 | HCID 24804837 | 110.1% |
Reaction Steps
A mixture of 4-benzyloxy-4′-(trifluoromethoxy)biphenyl-3-carbaldehyde (4.0 g, 9.336 mmol), malonic acid (2.137 g, 20.539 mmol), pyridine (4.3 ml) and piperidine (184 μl, 1.867 mmol) was refluxed for 1 hour under argon atmosphere. The reaction mixture was cooled to room temperature, adjusted to pH 1 by addition of 2N hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=1:1) to give the title compound (4.26 g, 97.0%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08044236B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-eb5734f85d104ffba084aa018856c50d |
| Source note | uspto-grants-2011_10 |