反应详情

温度

50 °C

A mixture of 1,1-dimethylethyl 4-[(2-amino-3-fluoro-5-methoxyphenyl)amino]-1-piperidinecarboxylate (D13a) (230 mg, 0.7 mmol), carbonyl diimidazole (150 mg, 1.0 mmol), and tetrahydrofuran (6 ml) was heated 1 h at 50° C. then partitioned between dichloromethane and water. The organic layer was purified by chromatography on silicagel eluting with 0 to 10% methanol in dichloromethane containing 0.2M ammonia to give the title compound as white crystals, 47%, 120 mg, M−−H=364.

1. customthen partitioned between dichloromethane and water
2. customThe organic layer was purified by chromatography on silicagel
3. washeluting with 0 to 10% methanol in dichloromethane containing 0.2M ammonia