Cl[P:2](Cl)Cl.[CH:5]1([Mg]Cl)[CH2:9][CH2:8][CH2:7][CH2:6]1.[CH:12]1(Cl)[CH2:16][CH2:15][CH2:14][CH2:13]1.[Mg].S(=O)(=O)(O)O.[C:24]1([CH3:30])[CH:29]=[CH:28][CH:27]=CC=1>O1CCCC1>[CH:5]1([P:2]([CH:24]2[CH2:29][CH2:28][CH2:27][CH2:30]2)[CH:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)[CH2:9][CH2:8][CH2:7][CH2:6]1A 200-ml four-necked flask sufficiently purged with nitrogen was equipped with a stirrer, a thermometer and a reflux condenser. 5.5 g (40 mmol) of trichlorophosphine and 40.0 ml of tetrahydrofuran were weighed in the flask. A cyclopentylmagnesium chloride solution was added dropwise to the flask at an internal temperature of 10-20° C. over a period of 3 hours, wherein the solution had been previously prepared from 13.8 g (132 mmol) of cyclopentyl chloride and 3.2 g (132 mmol) of metallic magnesium in 49 g of tetrahydrofuran. The mixture was stirred at 20-30° C. for 2 hours. Gas chromatography analysis confirmed the disappearance of trichlorophosphine. After the completion of the reaction, 61 ml of toluene was added, and 11.8 g (6 mmol) of 5% sulfuric acid was added dropwise to dissolve the magnesium salt, followed by separation. The organic phase was washed with 11.8 ml of water, and a solution of tricyclopentylphosphine was obtained.
불러오는 중…
