HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 4-Chloro-2-methyl-5-phenylisothiazol-3(2H)-one 1,1-dioxide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | HCID 68661656 | HCID 68661656 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4-Chloro-2-methyl-5-phenylisothiazol-3(2H)-one 1,1-dioxide | HCID 68662017 | 104% |
Reaktionsschritte
A solution of 4-chloro-5-phenylisothiazol-3(2H)-one 1,1-dioxide (2.0 g, 8.21 mmol) and MeI (3.5 g, 24.6 mmol) in DMF (30 ml) was cooled with an ice bath, and anhydrous potassium carbonate (1.13 g, 8.21 mmol) was added. The mixture was then allowed to warm to rt and stirred for 21 h. Water (60 ml) was added and the white precipitate formed, was filtered off and washed with water. Toluene was added to the precipitate and the mixture was evaporated and the residue was dried for three days under vacuum to give the title compound (2.2 g, 102%) containing traces of water and toluene. 1H NMR (400 MHz, CDCl3): δ 3.23 (s, 3H), 7.52-7.56 (m, 3H), 7.86-7.88 (m, 2H); 13C-NMR (100 MHz, CD3CN): δ 24.5, 123.8, 1291, 129.5, 130.7, 133.0, 143.1, 157.6.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07582629B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-45c600a773ac4635ba9a18c0d831f33a |
| Quellennotiz | uspto-grants-2009_09 |