HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → 3'-Chloro-4'-((methylsulfonyl)amino)acetophenone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Calcium hypochlorite | HCID 24504 | — |
| Edukt | N-(4-acetylphenyl)methanesulfonamide | HCID 684083 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3'-Chloro-4'-((methylsulfonyl)amino)acetophenone | HCID 19873458 | — |
Reaktionsschritte
To 2.13 g (10 mmole) of N-(4-acetylphenyl)methanesulfonamide in 50 ml of alcohol and 50 ml of water at 30° C. is added 1.43 g (10 mmol) of calcium hypochlorite. The solution is stirred for 24 hrs and an additional 1.43 g of calcium hypochlorite added. The mixture is stirred for 3 days at room temperature. The mixture is acidified with acetic acid to pH 6; concentrated and extracted into water-methylene chloride. The organic layer is dried, evaporated and the residue flash chromatographed on silica gel eluting in succession with 25% and 50% ethyl acetate-pet. ether. The solid product is recrystallized from Et2O-pet. ether; m.p. 129°-131° C. MW 247.71.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05155268 |
| Quelldatensatz | uspto-grants-1992_10 |
| ORD ID | ord-5a8495b24b8a4b4b991998f777e295bb |
| Quellennotiz | uspto-grants-1992_10 |