反应详情

温度

140 °C

A suspension of N-(2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}ethyl)-2,3,4-trifluoro-N-methylbenzamide (300 mg, 0.86 mmol), N-(1-ethyl-1H-pyrazol-3-yl)-3-hydroxy-5-{[(1S)-1-methyl-2-(methyloxy)ethyl]oxy}benzamide (290 mg, 0.91 mmol) and potassium carbonate (237 mg, 1.73 mmol) in DMA (20 mL) was heated to 140° C. for 4 hours. The reaction was poured into water (100 mL) and extracted with ethyl acetate (3×50 mL). The combined organic phases were washed with brine (50 mL) and dried (MgSO4), filtered and evaporated to give an orange oil. This was purified by column chromatography on alumina, eluting with 30-100% ethyl acetate in isohexane, to give the desired product as a colourless oil (300 mg).

1. extractionextracted with ethyl acetate (3×50 mL)
2. washThe combined organic phases were washed with brine (50 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customto give an orange oil
7. customThis was purified by column chromatography on alumina
8. washeluting with 30-100% ethyl acetate in isohexane