HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl 4-methoxyacetoacetate → HCID 54115946, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl 4-methoxyacetoacetate | HCID 123500 | — |
| Reactant | 3,4-Difluorobenzaldehyde | HCID 588088 | — |
| Reactant | Piperidinium acetate | HCID 3014295 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 54115946 | HCID 54115946 | 42,970.199% |
Reaction Steps
To a solution of methyl 4-methoxyacetoacetate (84.32 g, 0.577 mol), 3,4-difluorobenzaldehyde (82 g, 0.577 mmol), and piperidinium acetate (5.86 g, 0.068 mol) in benzene (1.5 L) 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 an oil (67 g, 47%). This product was a mixture of cis and trans isomers.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06172066B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-2f019379e9124518a3a1e9683211be2e |
| Source note | uspto-grants-2001_01 |