迪特-丁基(1,1-二苯丙胺-1-恩-2-基)磷烷

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

实验步骤: Into a reactor were introduced 1.37 g (5.0 mmol) of the 2-bromo-11-diphenylpropene obtained in Example 1 (2), 0.134 g (5.5 mmol) of magnesium, and 11 mL of THF under a nitrogen atmosphere. Iodine and bromobenzene were added to the mixture in a slight amount to ascertain initiation of a reaction. Thereafter, the reaction mixture was refluxed for 2 hours and then cooled. Thereto were added 0.520 g (5.3 mmol) of copper chloride and 1.1 mL (5.5 mmol) of chlorodi-t-butylphosphine. This reaction mixture was refluxed for 18 hours and then cooled to room temperature. Thereto was added 14 mL of heptane. The crystals yielded were taken out by filtration and dissolved in 40 mL of ethyl acetate. The resultant solution was washed with 28% ammonia water and an aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate. Thereafter, the solvent was removed under reduced pressure. The concentrate was recrystallized from ethanol to obtain 0.736 g (43%) of the target compound as white crystals. initiation of a reaction Thereafter, the reaction mixture was refluxed for 2 hours cooled This reaction mixture was refluxed for 18 hours The crystals yielded were taken out by filtration dissolved in 40 mL of ethyl acetate The resultant solution was washed with 28% ammonia water an aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate Thereafter, the solvent was removed under reduced pressure The concentrate was recrystallized from ethanol