反应详情

温度

105 °C

Under an argon atmosphere a mixture of the crude (R)-3-(5-bromo-2-fluoro-phenyl)-3-methyl-[1,4]oxazepan-5-one (626 mg, 1.2 mmol), sodium tert-butoxide (356 mg, 3.59 mmol), 2-di-tert-butylphosphino-2′,4′,6′-triisopropylbiphenyl (52.4 mg, 0.12 mmol), tris(dibenzylideneacetone)-dipalladium(0) chloroform adduct (38.3 mg, 0.036 mmol), and benzophenonimine (447 mg, 2.4 mmol) in toluene (15 ml) was heated at 105° C. for 16 hours in a sealed vial. For the workup, the reaction mixture was cooled to room temperature, evaporated at reduced pressure, and purified by chromatography on Silicycle-Si-amine column using a gradient of heptane and ethyl acetate=100/0 to 10/20 as the eluent. (R)-3-[5-(Benzhydrylidene-amino)-2-fluoro-phenyl]-3-methyl-[1,4]oxazepan-5-one (intermediate C12A) was obtained as a light yellow foam (348 mg, 69% of theory). MS (ISP): m/z=403.3 [M+H]+.

1. temperatureFor the workup, the reaction mixture was cooled to room temperature
2. customevaporated at reduced pressure
3. custompurified by chromatography on Silicycle-Si-amine column