HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 67418330, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | HCID 59186922 | HCID 59186922 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67418330 | HCID 67418330 | 99.4% |
Reaction Steps
3.32 g (15.43 mmol) of 4-formyl-3-(trifluoromethoxy)benzonitrile, 1.55 g (15.43 mmol) of 2,4-pentanedione, 1.39 g of acetic acid (23.15 mmol) and 262 mg (3.09 mmol) of piperidine are dissolved in 150 ml of dichloromethane and heated under reflux with an inverse water trap overnight. After complete conversion has been detected by a TLC check, the mixture is diluted with 100 ml of dichloromethane and washed with water and saturated sodium chloride solution. The solvent is removed in a rotary evaporator. 4.56 g (99% of theory) of crude 4-(2-acetyl-3-oxobut-1-en-1-yl)-3-(trifluoromethoxy)benzonitrile are obtained and are reacted directly without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08404709B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-161f6d299bce4fde838d9b19608509d4 |
| Source note | uspto-grants-2013_03 |