HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 1-Benzyl-3-(2-chloroethyl-methyl-amino)-pyrrolidine-2,5-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Benzylmaleimide | HCID 74204 | — |
| Edukt | Ethanamine, 2-chloro-N-methyl-, hydrochloride (1:1) | HCID 3028223 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 1-Benzyl-3-(2-chloroethyl-methyl-amino)-pyrrolidine-2,5-dione | HCID 15069998 | — |
Reaktionsschritte
74.8 g (0.4 mol) of N-benzylmaleimide [Arch. Pharm. 308, 489 (1975)] and 52.0 g (0.4 mol) of 2-chloroethyl-methylamine hydrochloride are initially introduced into 400 ml of dioxane and 40.4 g (0.4 mol) of triethylamine are added dropwise at 20° C. The mixture is then boiled under reflux for 5 hours. The batch is subsequently poured into 2 1 of ice-water and extracted with 3 portions of 400 ml of chloroform and the extract is washed with water, dried over sodium sulphate and concentrated on a rotary evaporator. Chromatography of the residue (101.1 g) on silica gel using ethyl acetate:petroleum ether (1:2) gives 56.8 g (51% of theory) of an oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05607942 |
| Quelldatensatz | uspto-grants-1997_03 |
| ORD ID | ord-f027df5983604d6e8bd77456a0611cbd |
| Quellennotiz | uspto-grants-1997_03 |