4-(4-FLUOROPHENYLSULFONYL)MORPHOLINE

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:87.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 4-[(4-fluorophenyl)sulfonyl]morpholine (0.25 g, 1 mmol), cesium carbonate (1.30 g, 4 mmol), and guanidine carbonate (1.08 g, 6 mmol) in 2 ml of 1-methyl-2-pyrrolidinone (NMP) is stirred at 85 to 90° C. for 24 hrs. It is then cooled to room temperature and diluted with ether. The resulting suspension is filtered, and the precipitate extracted with tetrahydrofuran (THF) to yield, after evaporation of solvent, 0.12 g of a yellow solid; mp 102-105° C.; MS (ESI) m/z 285.1 (M+H); HRMS: calcd for C11H16N4O3S, 284.0943; found (ESI_FT), 285.1011 (M+H). It is then cooled to room temperature The resulting suspension is filtered the precipitate extracted with tetrahydrofuran (THF) to yield after evaporation of solvent, 0.12 g of a yellow solid

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 4-fluorobenzenesulfonyl chloride (3.97 g, 20 mmol) in methylene chloride (40 ml), at 0° C., under nitrogen, with stirring, is added morpholine (4.4 mL, 50 mmol). The mixture is stirred at 0° C. for 15 min. and then warmed to room temperature for 18 hrs. The resulting suspension is filtered, and the filtrate is stirred with 10% potassium carbonate for 2 hrs. The methylene chloride is evaporated, and the aqueous suspension is filtered, and the precipitate is washed with water, and then dried in vacuo to give 5.0 g of a white solid; mp 106-107° C.; MS (APCI) m/z 246.1 (M+H). warmed to room temperature for 18 hrs The resulting suspension is filtered the filtrate is stirred with 10% potassium carbonate for 2 hrs The methylene chloride is evaporated the aqueous suspension is filtered the precipitate is washed with water dried in vacuo

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5 g of 4-fluorobenzenesulfonic acid morpholide were dissolved in 15 ml of N-methylpyrrolidone and mixed with 2.5 g of hydrazine hydrate, and the mixture was heated at 100° C. for 1 hour. After cooling to room temperature, 75 ml of water were added and the mixture was stirred at room temperature. After 2 hours, the solid was filtered off with suction and recrystallized from isopropanol. After cooling to room temperature the solid was filtered off with suction recrystallized from isopropanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 20 g of morpholine were added dropwise to a solution, cooled with ice, of 19.5 g of 4-fluorobenzenesulfonyl chloride in 100 ml of toluene, and the mixture was heated under reflux for 1 hour. After cooling, the mixture was concentrated under reduced pressure, the residue was stirred with water and the precipitate was filtered off with suction, washed with water and recrystallized from isopropanol. the mixture was heated under reflux for 1 hour After cooling the mixture was concentrated under reduced pressure the precipitate was filtered off with suction washed with water recrystallized from isopropanol