HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86644237, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Ethyl 4-chloroacetoacetate | HCID 69484 | — |
| Reactant | 5-(Aminomethyl)-2-chloropyridine | HCID 7020927 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86644237 | HCID 86644237 | 98% |
Reaction Steps
To a solution of 2.1 g of ethyl 4-chloroacetoacetate in 12 ml of toluene is added 0.15 ml of acetic acid. At 10° C.-30° C., with cooling, 2 g of 2-chloro-5-(aminomethyl)pyridine dissolved in 4 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. 4.2 g of ethyl 4-chloro-3-([[6-chloropyridin-3-yl]methyl]amino)but-2-enecarboxylate are obtained in a purity of 86% (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-7faf10a9caa946ffb0dc796bdeda86eb |
| Source note | uspto-grants-2013_07 |