HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Salicylamide → 2,2-dibutyl-4-oxo-2,3-dihydro-4H-1,3-benzoxazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Salicylamide | HCID 5147 | — |
| Edukt | 5-Nonanone | HCID 10405 | — |
| Edukt | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 2,2-dibutyl-4-oxo-2,3-dihydro-4H-1,3-benzoxazine | HCID 10084017 | 92,5% |
Reaktionsschritte
A mixture of 20 g of dibutylketone, 19.3 g of salicylamide and 2.7 g of p-toluenesulfonic acid monohydrate is added to 300 ml of toluene and the mixture is refluxed overnight by making use of a dehydrator of Dean Stark. After cooling, the reaction mixture is washed, dried and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; hexane:ethyl acetate =95:5) to obtain 34 g of 2,2-dibutyl-4-oxo-2,3-dihydro-4H-1,3-benzoxazine as a yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05442055 |
| Quelldatensatz | uspto-grants-1995_08 |
| ORD ID | ord-9efcac42f446489ba5cf5243c6c30bd3 |
| Quellennotiz | uspto-grants-1995_08 |