反应详情

温度

90 °C

A mixture of (6-chloro-2-methylsulfanyl-pyrimidin-4-yl)-[2-(3,4-dimethoxy-phenyl)-ethyl]-amine [250 mg, 0.74 mmol, Intermediate (31)], 3-hydroxy-benzoic acid ethyl ester (0.18 g, 1.1 mmol), and Cs2CO3 (0.48 g, 1.48 mmol) in DMF (4 mL) is heated to 90° C. for 15 h. The mixture is diluted with water, and extracted with EtOAc. The extracts are washed (water), dried (MgSO4), filtered, concentrated, and chromatographed (silica gel, 30% EtOAc in Heptane) to afford 3-{6-[2-(3,4-dimethoxy-phenyl)-ethylamino]-2-methylsulfanyl-pyrimidin-4-yloxy}-benzoic acid ethyl ester [0.29 g, 83%, Intermediate (71)]. LCMS: RT=3.7 minutes, MS: 470 (M+H).

1. extractionextracted with EtOAc
2. washThe extracts are washed (water)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customchromatographed (silica gel, 30% EtOAc in Heptane)