HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Difluorobenzaldehyde → HCID 54260394, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Difluorobenzaldehyde | HCID 588088 | — |
| Reactant | HCID 22570139 | HCID 22570139 | — |
| Catalyst | Piperidinium acetate | HCID 3014295 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 54260394 | HCID 54260394 | 92.2% |
Reaction Steps
To a solution of benzyl 4-methoxyacetoacetate (84 g, 0.37 mol), 3,4-difluorobenzaldehyde (52.5 g, 0.0.37 mmol), and piperidinium acetate (1.58 g, 2.63 mmol) in benzene (1L) were added molecular sieves (400 g) and the mixture was stirred at room temperature for 48 h. The molecular sieves were removed by filtration and the solvent was evaporated from the filtrate under reduced pressure. The residue was purified by column chromatography on silica gel using chloroform/ethyl acetate (100:3) to get the product as a white powder (118 g, 91%). The NMR showed this product to be a mixture of cis and trans isomers.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06228861B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-6ffda977e14142d7a164f15a5a789f74 |
| Source note | uspto-grants-2001_05 |