反应详情

Phenyl chloroformate (3.46 ml, 27.6 mmol) was added drop wise to a mixture of 6-amino-4-(thiophen-2-ylmethoxy)nicotinonitrile (intermediate 284, 2.90 g, 12.54 mmol) and pyridine (4.46 ml, 55.2 mmol) in THF (100 ml) at room temperature. The reaction mixture was stirred for 16 h at room temperature and then partitioned between EtOAc and saturated aqueous NaHCO3 solution, the organic layer washed with saturated brine, dried over MgSO4 and evaporated. The residue was purified by normal phase chromatography: 80 g RediSep® column, eluting with a gradient from heptane to EtOAc. Product containing fractions were combined and evaporated to give the title compound as a beige solid. (UPLC-MS 3) tR 1.14; ESI-MS 352.0 [M+H]+.

1. custompartitioned between EtOAc and saturated aqueous NaHCO3 solution
2. washthe organic layer washed with saturated brine
3. dry with materialdried over MgSO4
4. customevaporated
5. customThe residue was purified by normal phase chromatography
6. wash80 g RediSep® column, eluting with a gradient from heptane to EtOAc
7. additionProduct containing fractions
8. customevaporated