反应详情

To a solution of methyl 2-chloro-5-methanesulfonylbenzoate (23.4 g, 94 mmol) in toluene (250 ml) were added morpholine (9.8 ml, 113 mmol), cesium carbonate (40 g, 122 mmol), palladium acetate (380 mg, 1.4 mmol) and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (1.06 g, 1.7 mmol). After stirring overnight with heating under reflux, ethyl acetate (250 ml) was added. The organic layer was washed successively with water (200 ml×2) and saturated brine (200 ml), and dried over magnesium sulfate. Filtration and concentration gave methyl 5-methanesulfonyl-2-(morpholin-4-yl)benzoate as a crude product. The obtained compound was used for Step 4 without further purification.

1. temperaturewith heating
2. temperatureunder reflux
3. washThe organic layer was washed successively with water (200 ml×2) and saturated brine (200 ml)
4. dry with materialdried over magnesium sulfate
5. filtrationFiltration and concentration