HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Lutidine → HCID 19801961, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Ethyl 2,4-dichloro-4,4-difluorobutanoate | HCID 19801957 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19801961 | HCID 19801961 | 75% |
Reaction Steps
22.1 g of ethyl 2,4-dichloro-4,4-difluorobutyrate are dissolved in 100 ml of absolute tetrahydrofuran. 10.7 g of 2,6-dimethylpyridine and 2.0 g of 5% palladium/carbon catalyst are added and then gaseous hydrogen is passed in under atmospheric pressure until the hydrogen uptake is 100% of theory. The catalyst is removed by filtration and the tetrahydrofuran is removed by distillation and then the remaining oil is poured onto water, and the organic phase is separated off, dried with sodium sulfate, filtered and distilled under atmospheric pressure. 14.0 g of ethyl 4-chloro-4,4-difluorobutyrate are obtained in the form of a colourless oil of boiling point 154°-156° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05179121 |
| Source dataset | uspto-grants-1993_01 |
| ORD ID | ord-089e2fad318f4f48b86301028e60cdc8 |
| Source note | uspto-grants-1993_01 |