反应详情

温度

60 °C

A suspension of 4-(2-bromoethoxy)-3,5-difluorobenzonitrile (12 g, 45.8 mmol; see step (i) above), 9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester HCl-salt (11.5 g, 0.0435 mol; see WO 01/28992) and dry K2CO3 (25.32 g, 0.183 mol) in 140 mL of dry acetonitrile was stirred at 60° C. for five days under a nitrogen atmosphere. The reaction mixture was filtered through Celite® and the filtrate was then concentrated under reduced pressure. The residue was purified by column chromatography over silica gel, using 20% ethyl acetate in petroleum ether as eluent, to yield 12.55 g of the sub-title compound as a white solid.

1. filtrationThe reaction mixture was filtered through Celite®
2. concentrationthe filtrate was then concentrated under reduced pressure
3. customThe residue was purified by column chromatography over silica gel