反应详情

Benzyl isocyanate (1.2 g, Aldrich) was added at room temperature to a stirred solution of the product from step (b) (2.03 g) in toluene (25 ml). When addition was complete, the mixture was refluxed for 40 hours. The toluene was evaporated in vacuo and the residue flash chromatographed through a silica column using chloroform to give the desired product as a colourless oil which crystallised on standing (2.9 g). The product was recrystallised from IPA as fine white needles (1.8 g), mp 92°-93° C. The 200 MHz 1H NMR was consistent with the proposed structure.

1. additionWhen addition
2. temperaturethe mixture was refluxed for 40 hours
3. customThe toluene was evaporated in vacuo
4. customthe residue flash chromatographed through a silica column