HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 1-(1-Boc-4-piperidyl)-4-phenyl-3,1-benzoxazin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Triphosgene | HCID 94429 | — |
| Edukt | phenyl-(2-(1-Boc-4-piperidinylamino)phenyl) carbinol | HCID 57083091 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 1-(1-Boc-4-piperidyl)-4-phenyl-3,1-benzoxazin-2-one | HCID 22914669 | — |
Reaktionsschritte
Phenyl-(2-(1-Boc-4-piperidinylamino)phenyl) carbinol from Step 2 above (1.8 g, 4.7 mmol) was stirred in dry THF in an ice bath under nitrogen, and triphosgene (0.47 g, 1.57 mmol) was added followed by triethylamine (1.96 mL, 1.42 g, 14.1 mmol). The ice bath was removed and the mixture was stirred at ambient temperature for 18 hours. Water was added, and the mixture was extracted with ethyl acetate. The combined ethyl acetate fractions were washed with 1N HCl followed by saturated sodium bicarbonate, dried over sodium sulfate, filtered, and evaporated to dryness in vacuo to give 1-(1-Boc-4-piperidyl)-4-phenyl-3,1-benzoxazin-2-one.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05665719 |
| Quelldatensatz | uspto-grants-1997_09 |
| ORD ID | ord-9d66df4f5c6c4727b2ff08d02e8b5f85 |
| Quellennotiz | uspto-grants-1997_09 |