HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → Ethyl 5-methylpyridine-2-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Ethyl 2,3-dibromopropionate | HCID 97945 | — |
| Edukt | 1-Dimethylamino-1-aza-3-methyl-1,3-butadiene | HCID 86743903 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | Ethyl 5-methylpyridine-2-carboxylate | HCID 12243769 | — |
Reaktionsschritte
6.1 g of triethylamine are added at 0° C. to 13 g of ethyl 2,3-di-bromopropionate in 50 ml of dioxane. The mixture is stirred for 2 hours at room temperature and then a solution of 5.6 g of 1-dimethylamino-1-aza-3-methyl-1,3-butadiene and 6.1 g of triethylamine in 50 ml of dioxane is added dropwise. The reaction mixture is kept for 30 hours at 70° C. and then cooled and concentrated by evaporation. The residue is partitioned between water and ether and the organic phase is washed with brine, dried and concentrated by evaporation. The residue is distilled under reduced pressure, affording 3.2 g of the title compound as an oil with a boiling point of 69°-74° C. (at 0.08 mbar).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04923993 |
| Quelldatensatz | uspto-grants-1990_05 |
| ORD ID | ord-9a1d28c43bd94341a7846ecc45555c03 |
| Quellennotiz | uspto-grants-1990_05 |