HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Butylurea → N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-butyl-urea
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Butylurea | HCID 11595 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4-[2-(1-Oxo-isoindoline-2-carboxamido)-ethyl]-benzene sulfochloride | HCID 21162349 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-butyl-urea | HCID 21162325 | — |
Reaktionsschritte
4.8 g of butyl urea are dissolved in 100 ml of tetrahydrofurane and, while stirring, 1.5 g of 80% sodium hydride (in oil) are added. The mixture is heated for 3 hours to 60° C. whereupon 7.6 g of 4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzene-sulfochloride in 100 ml of tetrahydrofurane are added while cooling. The temperature is slowly raised to 60°-70° C. and stirring is continued at that temperature for 3 hours. The solvent is removed under reduced pressure, water is added to the residue, the mixture is filtered and the filtrate is acidified with dilute hydrochloric acid. After recrystallization from dilute acetone, the N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]benzenesulfonyl)-N'-butyl-urea melts at 189°-190° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04282239 |
| Quelldatensatz | uspto-grants-1981_08 |
| ORD ID | ord-eeaef196eedc4b268efebd985dfcd232 |
| Quellennotiz | uspto-grants-1981_08 |