反应详情

Phenyl chloroformate (3.89 ml, 31.0 mmol) was added drop wise to a mixture of 6-amino-4-isopropoxynicotinonitrile (intermediate 97, 2.5 g, 14.11 mmol) and pyridine (2.51 ml, 31.0 mmol) in THF (100 ml) at room temperature. The reaction mixture was stirred for 12 h at room temperature, additional pyridine (2.51 ml, 31.0 mmol) added, before stirring for an additional 12 h and then partitioned between EtOAc and saturated aqueous NaHCO3 solution. The organic layer was washed with saturated brine, dried over MgSO4 and evaporated. The residue was triturated with Et2O and the product obtained by filtration as a beige solid. (UPLC-MS 7) tR 1.09; ESI-MS 298.2 [M+H]+.

1. stirringbefore stirring for an additional 12 h
2. custompartitioned between EtOAc and saturated aqueous NaHCO3 solution
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over MgSO4
5. customevaporated
6. customThe residue was triturated with Et2O
7. customthe product obtained by filtration as a beige solid