反应详情

温度

50 °C

A solution containing 7-(aminomethyl)-7-methyl-3-neopentyl-1-oxa-3-azaspiro[4.5]decan-2-one (0.100 g, 0.373 mmol) in MeCN (5 mL) was treated with 4-chloro-2-fluoro-nitrobenzene (0.065 g, 0.373 mmol) and potassium carbonate (0.077 g, 0.559 mmol). The reaction mixture was heated to 50° C. and stirred for 18 h. Additional 4-chloro-2-fluoro-nitrobenzene (0.020 g, 0.114 mmol) was added, and the reaction was stirred at 50° C. for an additional 3 h. The reaction was cooled to rt and concentrated for purification on a 40 g silica gel column (0-100% EtOAc/hexanes, 25 min gradient; 40 mL/min elution; 254 nm detection) to afford the title compound (0.175 g, 100% yield). MS (m/z) 424.1 (M+H+).

1. stirringthe reaction was stirred at 50° C. for an additional 3 h
2. temperatureThe reaction was cooled to rt
3. concentrationconcentrated for purification on a 40 g silica gel column (0-100% EtOAc/hexanes, 25 min gradient; 40 mL/min elution; 254 nm detection)