HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lawesson's reagent → 6,11-Dihydro-N-(2,6-diisopropylphenyl)-2-methyldibenz[b,e]oxepin-11-carbothioamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lawesson's reagent | HCID 87949 | — |
| Edukt | Dibenz(b,e)oxepin-11-carboxamide, 6,11-dihydro-N-(2,6-bis(1-methylethyl)phenyl)-2-methyl- | HCID 3072807 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 6,11-Dihydro-N-(2,6-diisopropylphenyl)-2-methyldibenz[b,e]oxepin-11-carbothioamide | HCID 10455333 | 96,3% |
Reaktionsschritte
After 1.09 g of Compound 4 obtained in Example 4 was dissolved in 10 ml of toluene, 1.07 g of Lawesson's reagent was added to the solution. The mixture was heated under reflux for an hour. The reaction mixture was allowed to stand at room temperature, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (2:1)] to obtain 1.46 g of a crude product. The crude product was recrystallized from ethyl acetate-hexane to obtain 1.09 g of Compound 36.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05478835 |
| Quelldatensatz | uspto-grants-1995_12 |
| ORD ID | ord-ab9b161e45c343ca9daa8c8693bf846c |
| Quellennotiz | uspto-grants-1995_12 |