HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Bicarbonate → 1-(2-Fluoro-5-methylsulfonylphenyl)piperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Bis(2-chloroethyl)amine hydrochloride | HCID 522769 | — |
| Edukt | 2-Fluoro-5-(methylsulfonyl)aniline | HCID 2774637 | — |
| Lösungsmittel | 1,2-Dichlorobenzene | HCID 7239 | — |
| Produkt | 1-(2-Fluoro-5-methylsulfonylphenyl)piperazine | HCID 22032011 | 39% |
Reaktionsschritte
10 mL solution of 432 mg 2-fluoro-5-methylsulfonylphenylamine (compound in Production Example 338) and 490 mg bis(2-chloroethyl)amine hydrochloride in 1,2-dichlorobenzene was stirred at 200° C. for 9 hours. The reaction mixture was neutralized by adding an aqueous saturated sodium bicarbonate solution and then extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate, the solvent was removed, and the resulting crude product was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 230 mg of the title compound (dark brown solid).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07074801B1 |
| Quelldatensatz | uspto-grants-2006_07 |
| ORD ID | ord-301e0a8a384a44118b2bb5ca131ee775 |
| Quellennotiz | uspto-grants-2006_07 |