HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86644238, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Ethyl 4-chloroacetoacetate | HCID 69484 | — |
| Reactant | 2,2-Difluoroethanamine | HCID 136274 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86644238 | HCID 86644238 | 98% |
Reaction Steps
To a solution of 197.2 g of ethyl 4-chloroacetoacetate in 1080 ml of toluene are added 13.3 ml of acetic acid. At 10° C.-30° C., with cooling, 100 g of 2,2-difluoroethylamine dissolved in 360 ml of ethanol are added dropwise. Subsequently, the mixture is stirred at room temperature for 8 h and the solvent is removed under reduced pressure at temperatures of down to 35° C. 278 g of ethyl 4-chloro-3-(2,2-difluoroethylamino)but-2-enecarboxylate are obtained in a purity of 93% (this corresponds to 98% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08487112B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-edd077b62c064a4c94acad7627430e41 |
| Source note | uspto-grants-2013_07 |