HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethyl-p-toluidine → 6,8-Dichloro-3-(5-cyclopropyl-[1,2,4]oxadiazol-3-yl)-4H-2,5,10b-triaza-benzo[e]azulene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethyl-p-toluidine | HCID 7471 | — |
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | HCID 22713497 | HCID 22713497 | — |
| Lösungsmittel | Chlorobenzene | HCID 7964 | — |
| Produkt | 6,8-Dichloro-3-(5-cyclopropyl-[1,2,4]oxadiazol-3-yl)-4H-2,5,10b-triaza-benzo[e]azulene | HCID 22713545 | 63% |
Reaktionsschritte
8-Chloro-3-(5-cyclopropyl-[1,2,4]oxadiazol-3-yl)-4,5-dihydro-2,5,10b-triaza-benzo[e]azulen-6-one (0.84 g, 2.5 mmol) was suspended in chlorobenzene (8 mL), N,N-dimethyl-p-toluidine (1.1 mL, 7.4 mmol) and phosphorus oxychloride (0.34 mL, 3.7 mmol) were added and the mixture was refluxed overnight. The resulting solution was evaporated and the residue was purified by chromatography on silica gel in CH2Cl2/acetone 10:1. One obtained a white solid (0.56 g, 63%). mp 200° C. m/z 359(M).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06743789B2 |
| Quelldatensatz | uspto-grants-2004_06 |
| ORD ID | ord-80f739d1ea654a9eb6c80e6283701e33 |
| Quellennotiz | uspto-grants-2004_06 |