反应详情

温度

115 °C

Potassium carbonate (1.00 g) was added to a solution of 3-hydroxy-5-{[(1S)-2-hydroxy-1-methylethyl]oxy}-N-(1-methyl-1H-pyrazol-3-yl)benzamide (1.41 g) and 1-chloro-4,5-difluoro-2-(methylsulfonyl)benzene (0.79 g) in NMP (20 mL). The mixture was heated to 115° C. for 3.5 hours and left to cool before being poured into water (300 mL) and extracted with ethyl acetate (2×150 mL). The combined organics were washed with water, brine and dried (MgSO4) before evaporation in vacuo. Chromatography on silica, eluting with 0 to 10% methanol in ethyl acetate, afforded the desired compound (0.86 g)

1. waitleft
2. temperatureto cool
3. extractionextracted with ethyl acetate (2×150 mL)
4. washThe combined organics were washed with water, brine
5. dry with materialdried (MgSO4)
6. custombefore evaporation in vacuo
7. washChromatography on silica, eluting with 0 to 10% methanol in ethyl acetate