HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide diethylacetal → 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide diethylacetal | HCID 70913 | — |
| Edukt | Ethyl 3-pyridylacetate | HCID 96490 | — |
| Produkt | 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester | HCID 68704864 | — |
Reaktionsschritte
37.4 g (226 mmol) of ethyl pyridin-3-ylacetate in 100 g (679 mmol) of dimethylformamide diethyl acetal are heated at 100° C. overnight. After cooling, the mixture is concentrated and the residue is initially pre-purified by flash chromatography on silica gel (mobile phase: gradient cyclohexane/ethyl acetate 1:1 ethyl acetate/ethanol 9:1). The product obtained in this manner is then subjected to fine purification by distillation under reduced pressure (1 mbar, bath temperature 200° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08524699B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-2fab76d5241947dead68d408eaf254c6 |
| Quellennotiz | uspto-grants-2013_09 |