HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dicyclohexylcarbodiimide → (S)-tert-butyl 1-(3-(4-chlorophenyl)-1,2,4-oxadiazol-5-yl)ethylcarbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Edukt | Tert-butoxycarbonylalanine | HCID 85082 | — |
| Edukt | 4-chloro-N'-hydroxybenzenecarboximidamide | HCID 224650 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | (S)-tert-butyl 1-(3-(4-chlorophenyl)-1,2,4-oxadiazol-5-yl)ethylcarbamate | HCID 90414461 | 48% |
Reaktionsschritte
A solution of 4-chloro-N′-hydroxybenzimidamide (1.24 g, 7.27 mmol), (S)-2-(tert-butoxycarbonylamino)propanoic acid (1.38 g, 7.27 mmol, 1.0 equiv), and DCC (1.65 g, 8.00 mmol, 1.1 equiv) in 1,4-dioxane (73 mL) was heated at 100° C. for 18 hours. The reaction was then cooled to room temperature and concentrated in vacuo. Silica gel column chromatography (EtOAc/Heptane, 0 to 35%) provided (S)-tert-butyl 1-(3-(4-chlorophenyl)-1,2,4-oxadiazol-5-yl)ethylcarbamate (1.13 g, white solid) in 48% yield. 1H NMR (400 MHz, CDCl3) δ 8.03 (d, J=8.8 Hz, 2H), 7.47 (d, J=8.8 Hz, 2H), 5.18 (m, 1H), 1.64 (d, J=6.8 Hz, 3H), 1.47 (s, 9H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09434719B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-d3f5ba6193aa4df5b32f016183bb543e |
| Quellennotiz | uspto-grants-2016_09 |