反应详情

7.2 g of the product of Stage A, 6.5 g of anhydrous potassium carbonate and 1.48 ml of n-propyl isocyanate were stirred in 180 ml of acetone at reflux for 2 hours 30 minutes. After cooling, the solution was treated with 2N hydrochloric acid and the residue obtained was dissolved in an aqueous mixture of dichloromethane. After extraction with methylene chloride, the extracts were dried and the solvents were eliminated under reduced pressure and the product was crystallized from ethyl acetate to obtain 6.5 g of the expected product as a white solid with a Rf (SiO2, ethyl acetate)=0.48 and melting at 131°-133° C.

1. temperatureat reflux for 2 hours 30 minutes
2. temperatureAfter cooling
3. customthe residue obtained
4. extractionAfter extraction with methylene chloride
5. customthe extracts were dried
6. customthe product was crystallized from ethyl acetate