HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl iodide → 1-(4-Acetylamino-5-chloro-2-methoxyphenyl)-5-chloropentan-1-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-(4-Acetylamino-5-chloro-2-hydroxyphenyl)-5-chloropentan-1-one | HCID 19081879 | — |
| Lösungsmittel | Methyl Ethyl Ketone | HCID 6569 | — |
| Produkt | 1-(4-Acetylamino-5-chloro-2-methoxyphenyl)-5-chloropentan-1-one | HCID 19081861 | 67,7% |
Reaktionsschritte
1-(4-Acetylamino-5-chloro-2-hydroxyphenyl)-5-chloropentan-1-one (1.07 g, 3.5 mmol), potassium carbonate (1.38 g, 10.0 mmol) and iodomethane (0.62 mL, 10.0 mmol) were combined in methyl ethyl ketone (20 mL) and stirred at reflux temperature for 4 hours, 15 minutes. The mixture was partitioned between ethyl acetate and water. The ethyl acetate layer was separated, washed in brine, dried over sodium sulfate, and then evaporated to leave a solid residue. Crystallization of the residue from ethyl acetate-hexanes gave 1-(4-acetylamino-5-chloro-2-methoxyphenyl)-5-chloro-pentan-1-one (0.720 g, 2.37 mmol), m.p. 98°-100° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05763458 |
| Quelldatensatz | uspto-grants-1998_06 |
| ORD ID | ord-12c40d93e8884fb3b03071ddda14a120 |
| Quellennotiz | uspto-grants-1998_06 |