HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 54488685, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Methyl acetoacetate | HCID 7757 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | 3-Chloro-4-(trifluoromethyl)benzaldehyde | HCID 19031287 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54488685 | HCID 54488685 | — |
Reaction Steps
32.3 g (155 mol) of 3-chloro-4-trifluoromethylbenzaldehyde and 18.0 g (155 mmol) of methyl acetoacetate are dissolved in 200 ml of methylene chloride, and 1.2 ml of piperidine and 1 ml of glacial acetic acid are added. The mixture is heated for 5 hours, using a water separator. It is then washed with water, dried over MgSO4 and concentrated. The product is recrystallized twice from methanol. 25.6 g (54% of theory) of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05652251 |
| Source dataset | uspto-grants-1997_07 |
| ORD ID | ord-c1eb2cf0952d4468be77ee164877a79e |
| Source note | uspto-grants-1997_07 |