反应详情

温度

160 °C

A mixture of 7,8-difluoro-4-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (725 mg, 2.0 mmol), 3-hydroxy-5-[(1S)-2-methoxy-(1-methylethyl)oxy]-N-(1-methyl-1H-pyrazol-3-yl)benzamide (600 mg, 1.97 mmol) and potassium carbonate (550 mg, 3.88 mmol) in DMA (10 mL) was heated to 160° C. for 5 hours. Water (20 mL) was added to the reaction and extracted with ethyl acetate (3×30 mL). The combined organic phases were washed with water (2×30 mL) and brine (2×30 mL), dried (MgSO4), filtered and evaporated to give a yellow oil. This was purified by column chromatography on silica, eluting with 20-100% ethyl acetate in isohexane, to give the desired compound as a foam (65 mg).

1. extractionextracted with ethyl acetate (3×30 mL)
2. washThe combined organic phases were washed with water (2×30 mL) and brine (2×30 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customto give a yellow oil
7. customThis was purified by column chromatography on silica
8. washeluting with 20-100% ethyl acetate in isohexane