HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Butanol → 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Butanol | HCID 263 | — |
| Edukt | Dibutyl carbonate | HCID 68333 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Edukt | HCID 15557308 | HCID 15557308 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Produkt | 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one | HCID 15557326 | — |
Reaktionsschritte
A mixture of 3-hydroxy-3-isopropylaminomethyl-3,4-dihydro-2H-1,5-benzodioxepin (11.85 g.; 50 millimoles), prepared as described in Example 1, and dibutyl carbonate (13.1 g.) with a small piece of metallic sodium is heated in an oil bath. The temperature then is slowly raised to 170° C. with removal of butanol. Finally, the mixture is heated between 170°-200° C. with removal of excess dibutyl carbonate. The cooled reaction product is dissolved in benzene, washed with water, dried over sodium sulfate, and the solvent evaporated to give 3'-isopropyl-3,4-dihydro-2H-1,5-benzodioxepin-3-spiro-5'-oxazolidin-2'-one, m.p. 121°-122° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US03944560 |
| Quelldatensatz | uspto-grants-1976_03 |
| ORD ID | ord-baf10c7490ea425cbcdd0e469640b157 |
| Quellennotiz | uspto-grants-1976_03 |