HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Selenium Dioxide → 3-Hydroxy-6-methylpyridine-2-carbaldehyde
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Selenium Dioxide | HCID 24007 | — |
| Edukt | 3-Hydroxy-2-hydroxymethyl-6-methylpyridine | HCID 135128 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 3-Hydroxy-6-methylpyridine-2-carbaldehyde | HCID 12421986 | 57,3% |
Reaktionsschritte
3-Hydroxy-6-methyl-2-pyridine methanol (20.0 g, 0.14 mol) and selenium dioxide(8.0 g, 72 mmol) were dissolved in 140 mL of 1,4-dioxane and 280 mL of absolute ethanol. The resulting mixture was heated at 80°-85° C. for 12 h. The selenium precipitate was removed by filtration and the filtrate was concentrated to dryness in vacuo. The dark red residue was sublimed at 90° C. and 14 mmHg for 6 h to obtain 11.0 g (56%) of pure product, m.p. 101°-102° C.; 1H NMR (CDCl3) δ: 10.50 (br s, 1H), 10.03 (s, 1H), 7.27 (s, 2H); 2.53 (s, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05290942 |
| Quelldatensatz | uspto-grants-1994_03 |
| ORD ID | ord-78476dc1c0804450a72973a1fefc0b35 |
| Quellennotiz | uspto-grants-1994_03 |