HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
tert-Butanol → tert-Butyl (2-cyanopyridin-4-yl)carbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | tert-Butanol | HCID 6386 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Edukt | 2-Cyanoisonicotinic Acid | HCID 2762513 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | tert-Butyl (2-cyanopyridin-4-yl)carbamate | HCID 22939607 | — |
Reaktionsschritte
While stirring at room temperature, 1.8 ml of triethylamine and 2.8 ml of DPPA were added in that order to 100 ml of t-butanol solution containing 1.5 g of 2-cyanoisonicotinic acid, and the mixture was heated under refulx for 4 hours and 25 minutes. The reaction mixture was cooled to room temperature, mixed with water and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate and dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by a silica gel column chromatography, and 1.34 g of the title compound was obtained from ethyl acetate-hexane (1:2, v/v) eluate.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06673799B1 |
| Quelldatensatz | uspto-grants-2004_01 |
| ORD ID | ord-d792eb831adb4ae8936f7104c890d60a |
| Quellennotiz | uspto-grants-2004_01 |