Reaktion #2168845
ord-1888fc7206f54f62a49636f9af4733d4
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturthe mixture refluxed for 30 minutes or until solution
- 2Temperaturreflux
- 3Temperaturto cool
- 4Einengenconcentrated
- 5workup.ADDITIONdiluted with water (20 mL)
- 6Filtrationfiltered
- 7Waschenthe solid columned on silica gel, eluting with 20% ethyl acetate in hexanes (loaded in chloroform)
Vorschrift
Triethylamine (1.67 g, 0.017 mol) was added to a solution of the compound prepared in Step 2 above (4.0 g, 0.015 mol) in acetonitrile (200 mL) and the mixture refluxed for 30 minutes or until solution becomes homogeneous. 2,6-Diisopropylphenyl isocyanate (3.71 g, 0.018 mol) was then added and reflux continued for 18 hours. The mixture was allowed to cool, concentrated, diluted with water (20 mL), filtered, and the solid columned on silica gel, eluting with 20% ethyl acetate in hexanes (loaded in chloroform) to give 0.54 g of a solid; m.p 114°-116.5° C.