反应详情

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.

1. temperaturethe mixture refluxed for 30 minutes or until solution
2. temperaturereflux
3. temperatureto cool
4. concentrationconcentrated
5. additiondiluted with water (20 mL)
6. filtrationfiltered
7. washthe solid columned on silica gel, eluting with 20% ethyl acetate in hexanes (loaded in chloroform)