HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 5-Methylnicotinonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Trifluoroacetic anhydride | HCID 9845 | — |
| Edukt | 5-Methylpyridine-2-carboxamide | HCID 12362937 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 5-Methylnicotinonitrile | HCID 637838 | 100,9% |
Reaktionsschritte
To a suspension of 5-methylpyridinylcarboxamide from step 2 (10.5 g, 0.077 mol) in triethylamine (23.3 g, 0.23 mol) and 400 mL of methylene chloride was added trifluoroacetic anhydride (21.0 g, 0.100 mol) rapidly at 0° C. The reaction was completed after a few minutes. Water was added and the aqueous layer was extracted with methylene chloride. The combined organic layers were washed with water, brine and dried over magnesium sulfate. After filtration, the filtrate was concentrated to give 9.18 g of 3-cyano-5-methylpyridine crude, which was used in the next step without purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06613789B2 |
| Quelldatensatz | uspto-grants-2003_09 |
| ORD ID | ord-d1c3b91e71484f2d82642aba7926461a |
| Quellennotiz | uspto-grants-2003_09 |