HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benzoic acid, 2-chloro-5-(chlorosulfonyl)- → 2-Chloro-5-(4-hydroxymethylpiperidinosulfonyl)benzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benzoic acid, 2-chloro-5-(chlorosulfonyl)- | HCID 67306 | — |
| Edukt | 4-Piperidinemethanol | HCID 420771 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-Chloro-5-(4-hydroxymethylpiperidinosulfonyl)benzoic acid | HCID 20505867 | — |
Reaktionsschritte
2-Chloro-5-chlorosulfonylbenzoic acid (5.0 g.) is added to a solution of 4-piperidyl carbinol (6.9 g.) in 40 ml. of methylene chloride. The solution is refluxed for 2 hours, cooled to room temperature and stirred overnight. The solution is evaporated to dryness, the gummy residue dissolved in 1 N sodium hydroxide, and the alkaline solution extracted twice with ether. The aqueous solution is acidified with concentrated hydrochloric acid, and the precipitate recovered by filtration. Recrystallization from ethyl acetate yields crystals, m.p. 185°-187° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04377521 |
| Quelldatensatz | uspto-grants-1983_03 |
| ORD ID | ord-37bfdf2cf16e4d66871ca50ca34985de |
| Quellennotiz | uspto-grants-1983_03 |