HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosgene → 1-chloro-N-(2-chloro-4-fluoro-5-isocyanatophenyl)methanesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosgene | HCID 6371 | — |
| Edukt | N-(5-amino-2-chloro4-fluorophenyl)-1-chloromethanesulfonamide | HCID 11000212 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 1-chloro-N-(2-chloro-4-fluoro-5-isocyanatophenyl)methanesulfonamide | HCID 11077402 | 95,5% |
Reaktionsschritte
To a stirred solution of phosgene (68 mmol) in 35 mL toluene was added the title compound of Step D (4.2 g, 15.4 mmol) in 80 mL toluene at 0° C. and the reaction was stirred at room temperature overnight. The temperature was then raised to 70° C. for 4 h. After cooling to room temperature, the reaction mixture was filtrated and the solvent was removed under reduced pressure. Drying of the white precipitate under reduced pressure yielded the title compound of Step E (4.4 g, 95%) melting at 101.5-102.5° C. 1H NMR (CDCl3) δ 7.5 (d, 1H), 7.3 (d, 1H), 7.0-6.9 (br s, 1H), 4.64.5 (s, 2H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06060432 |
| Quelldatensatz | uspto-grants-2000_05 |
| ORD ID | ord-876da175843b498091fe36facd3e0ee5 |
| Quellennotiz | uspto-grants-2000_05 |