反应详情

To a stirred solution of Intermediate 5 (2.0 g) in dichloromethane (100 ml) was added 4-chlorophenylisocyanate (1.35 g). The mixture was stirred at 22° C. for 18 h before 10% 0.880 ammonia solution in methanol (10 ml) was added. Stirring was continued for a further 30 min before the solvent was removed in vacuo. The residue was purified by Biotage flash chromatography on silica gel, eluting with 33% ethyl acetate/cyclohexane; further purification by Biotage flash chromatography on silica gel, eluting with 500:8:1 dichloromethane/ethanol/0.880 ammonia solution gave the impure title compound as a buff solid (3.6 g).

1. additionwas added
2. customwas removed in vacuo
3. customThe residue was purified by Biotage flash chromatography on silica gel
4. washeluting with 33% ethyl acetate/cyclohexane
5. customfurther purification by Biotage flash chromatography on silica gel
6. washeluting with 500:8:1 dichloromethane/ethanol/0.880 ammonia solution