HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86644230, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Ethyl 4-chloroacetoacetate | HCID 69484 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86644230 | HCID 86644230 | 92% |
Reaction Steps
To a solution of 300 of ethyl 4-chloroacetoacetate in 519 ml of toluene and 200 ml of ethanol are added 20.8 ml of acetic acid. At 10° C.-30° C., with cooling, 188.7 g of a 33% methylamine solution in 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. 328 g of ethyl 4-chloro-3-(methylamino)but-2-enecarboxylate are obtained in a purity of 91% (this corresponds to 92% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08487112B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-bbc57b59f79143808d53312bca74def6 |
| Source note | uspto-grants-2013_07 |