反应详情

温度

65 °C

A mixture of 3-bromo-6-fluoro-N-(2-hydroxyethyl)-N-(4-methoxybenzyl)-2-methylbenzamide (130b, 5.00 g, 12.6 mmol) and Cs2CO3 (8.20 g, 25.3 mmol) in dry DMF (60 mL) was stirred at 65° C. for 14 hours. To the reaction mixture was added brine (100 mL). The mixture was extracted with EtOAc (2×50 mL). The combined organic layers were washed with brine (4×60 mL), dried over Na2SO4, and concentrated under vacuum. The residue was purified by column chromatography (petroleum ether/EtOAc, 5/1) to give 7-bromo-4-(4-methoxybenzyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (130c, 2.8 g, 59%) as a colorless oil.

1. extractionThe mixture was extracted with EtOAc (2×50 mL)
2. washThe combined organic layers were washed with brine (4×60 mL)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under vacuum
5. customThe residue was purified by column chromatography (petroleum ether/EtOAc, 5/1)