反应详情

温度

160 °C

Caesium carbonate (523 mg) was added to a solution of 3-hydroxy-5-{[(1S)-2-hydroxy-1-methylethyl]oxy}-N-(1-methyl-1H-pyrazol-3-yl)benzamide (234 mg) and 1,2,4-trifluoro-5-(methylsulfonyl)benzene (169 mg) in acetonitrile (5 mL) was added. The mixture was heated in a sealed microwave vial to 160° C. for 7000 seconds and left to cool before being filtered and washed with acetonitrile (10 mL). The filtrate was evaporated in vacuo and chromatographed on silica, eluting with 0 to 10% methanol in ethyl acetate. This gave incomplete resolution so the mixture was purified by preparatory HPLC using a gradient of 5 to 95% acetonitrile in water to afford the desired compound (5.1 mg)

1. additionwas added
2. waitleft
3. temperatureto cool
4. filtrationbefore being filtered
5. washwashed with acetonitrile (10 mL)
6. customThe filtrate was evaporated in vacuo
7. customchromatographed on silica
8. washeluting with 0 to 10% methanol in ethyl acetate
9. customThis gave incomplete resolution so the mixture was purified by preparatory HPLC