反应详情

To a solution of N-[4-(2-chloro-phenyl)-pyridin-3-yl]-N-methyl-5-trifluoromethyl-isophthalamic acid methyl ester (200 mg, 446 μM, example 75) in THF (3.3 mL) were added methyl magnesium bromide (1M solution in butyl ether, 1.6 mL, 1.56 mmol) within 2 min. The reaction was poured on EtOAc (20 mL) and aqueous sodium potassium tartrate solution (20 mL) and the phases were separated. The aqueous phase was extracted with EtOAc (20 mL) and the combined organic phases were washed with brine, dried over magnesium sulfate, filtered and evaporated. The compound was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane:EtOAc (100:0 to 0:100). Colorless solid (115 mg, 57%). MS (ESI): m/z=449.123 [M+H]+.

1. customthe phases were separated
2. extractionThe aqueous phase was extracted with EtOAc (20 mL)
3. washthe combined organic phases were washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customevaporated
7. customThe compound was purified by silica gel chromatography
8. washeluting with a gradient of n-heptane:EtOAc (100:0 to 0:100)