叔丁基二苯基磷

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

实验步骤: 466 ml of a 1.06 Molar titrated solution of 494 mmoles of t-butylmagnesium chloride in 466 ml of ether was added dropwise to a stirred solution of 88.4 g (494 mmoles) of phenyldichlorophosphine in 750 ml of anhydrous ether, maintained at +10° C. under an inert atmosphere. After the addition was complete the mixture was stirred for 15 minutes at +10° C., then the reaction mixture was allowed to gradually warm to ambient temperature. A Grignard mixture of 741 mmoles of phenylmagnesium bromide (prepared from 116.4 g of bromobenzene and 19.8 g of magnesium turnings in 450 ml of anhydrous ether) was added dropwise at +27° C., and the reaction mixture was then refluxed for 18 hours. The mixture was cooled to +18° C., and 340 ml of water was added dropwise at a temperature of between +18° C. and +36° C. After treatment with concentrated hydrochloric acid and ammonium hydroxide distillation gives t-butyldiphenylphosphine. 31P-NMR(delta)=17.53 ppm (relative intensity 1000.59), Yield=about 46%, BP=120°-125° C. at 0.2 torr. maintained at +10° C. under an inert atmosphere After the addition was added dropwise at +27° C. the reaction mixture was then refluxed for 18 hours The mixture was cooled to +18° C. After treatment with concentrated hydrochloric acid and ammonium hydroxide distillation

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

实验步骤: 466 ml of a 1.06 Molar titrated solution of 494 mmoles of t-butylmagnesium chloride in 466 ml of ether was added dropwise to a stirred solution of 88.4 g (494 mmoles) of phenyldichlorophosphine in 750 ml of anhydrous ether, maintained at +10° C. under an inert atmosphere. After the addition was complete the mixture was stirred for 15 minutes at +10° C., then the reaction mixture was allowed to gradually warm to ambient temperature. A Grignard mixture of 741 mmoles of phenylmagnesium bromide (prepared from 116.4 g of bromobenzene and 19.8 g of magnesium turnings in 450 ml of anhydrous ether) was added dropwise at +27° C., and the reaction mixture was then refluxed for 18 hours. The mixture was cooled to +18° C., and 340 ml of water was added dropwise at a temperature of between +18° C. and +36° C. After treatment with concentrated hydrochloric acid and ammonium hydroxide distillation gives t-butyldiphenylphosphine. 31P-NMR(delta)=17.53 ppm (relative intensity 1000.59), Yield=about 46%, BP=120°-125° C. at 0.2 torr. maintained at +10° C. under an inert atmosphere After the addition was added dropwise at +27° C. the reaction mixture was then refluxed for 18 hours The mixture was cooled to +18° C. After treatment with concentrated hydrochloric acid and ammonium hydroxide distillation