反应 #3243185
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05565543
反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Anhydrous nickel(II) chloride (60 mg, 0.46 mmole), triphenylphosphine (800 mg, 3.05 mmole), sodium iodide (180 mg, 1.2 mmole), and activated zinc powder (1.2 g, 18 mmole) are placed into a 25 ml flask under an inert atmosphere along with 7 ml of anhydrous N-methylpyrrolidinone (NMP). This mixture is stirred at 50° C. for about 10 minutes, leading to a deep-red coloration. A solution of 3.4 g (11.5 mmole) of 2,5-dichlorobenzenesulfonylmorpholine, which is prepared by the reaction of 2,5-dichlorobenzenesulfonyl chloride with morpholine, in 8 ml of anhydrous NMP is then added by syringe. After stirring for 60 hours, the resulting highly viscous solution is poured into 100 ml of 1 molar hydrochloric acid in ethanol to dissolve the excess zinc metal and to precipitate the polymer. This suspension is filtered and triturated with acetone to afford, after isolation and drying, solid polyparabenzenesulfonylmorpholine. is then added by syringe After stirring for 60 hours to precipitate the polymer This suspension is filtered triturated with acetone to afford after isolation and drying
来源 ID: ord-5e47dda1d0974507bbb66b6890277608