HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Pyridine → 5-(2-chloro-6-fluorophenyl)-2-(4-iodophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Phosgene | HCID 6371 | — |
| Edukt | HCID 117965459 | HCID 117965459 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | 5-(2-chloro-6-fluorophenyl)-2-(4-iodophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 136644854 | 41,7% |
Reaktionsschritte
The title a compound was prepared according to the procedure described in step-4 of Intermediate-1 using 2-chloro-6-fluoro-N′-(4-iodophenyl)benzene carbohydrazonamide (0.900 g, 2.31 mmol), pyridine (0.65 mL, 5.79 mmol), phosgene (2.50 mL, 4.63 mmol) and CHCl3 (20 mL). The obtained crude product was purified with column chromatography on silica gel eluting with 1.0% MeOH:DCM to afford 0.400 g of the desired product. 1H NMR (300 MHz, DMSO d6): δ 7.47 (t, J=9.0 Hz, 2H), 7.54-7.82 (m, 5H), 12.62 (s, 1H). MS (m/z): 414.25 (M−H)−.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09096545B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-f91d892154244da8b1780d90543b311d |
| Quellennotiz | uspto-grants-2015_08 |