反应详情

To a solution of 4-(4-fluoro-2-methoxyphenyl)-N-(2-(methylsulfonyl)ethyl)pyridin-3-amine (0.08 g, 247 μmol, example 192, intermediate a) and 3-(methylsulfonyl)-5-(trifluoromethyl)benzoyl chloride (177 mg, 617 μmol, example 223, intermediate d) in CH2Cl2 (2 mL) was added DIPEA (128 mg, 172 μL, 987 μmol) and the clear solution was stirred at room temperature for 19 hours. The reaction mixture was poured on saturated aqueous NH4Cl solution and CH2Cl2 and the layers were separated. The aqueous layer was extracted twice with CH2Cl2. The organic layers were dried over MgSO4, filtered, treated with silica gel and evaporated. The compound was purified by silica gel chromatography on a 20 g column using a MPLC system eluting with a gradient of n-heptane:EtOAc (100:0 to 0:100). Light brown foam (0.075 g; 52%). MS (ESI): m/z=575.09 [M+H]+.

1. customthe layers were separated
2. extractionThe aqueous layer was extracted twice with CH2Cl2
3. dry with materialThe organic layers were dried over MgSO4
4. filtrationfiltered
5. additiontreated with silica gel
6. customevaporated
7. customThe compound was purified by silica gel chromatography on a 20 g column
8. washeluting with a gradient of n-heptane:EtOAc (100:0 to 0:100)