一羰基二氢三(三苯基膦)合钌的合成及表征

SYNTHESIS AND CHARACTERIZATION OF CARBONYLDIHYDRIDOTRIS(TRIPHENYLPHOSPHINE) RUTHENIUM

在碱性条件下,由三氯化钌、三苯基膦与甲醛溶液反应制备了一羰基二氢三(三苯基膦)[RuH_2(CO) (Ph_3P)_3]。考察了三苯基膦、甲醛溶液、碱的种类及用量和溶剂种类及用量、反应时间等对反应的影响。结果表明,在氮气保护、反应温度78℃、氢氧化钾存在条件下,n(三氯化钌):n(三苯基膦):n(甲醛溶液)=1:6:160,乙醇为溶剂,反应时间2 h,RuH_2(CO)(Ph_3P)_3收率可以达到84%以上。对所得的目标产物进行了IR,~1H NMR,^(13)CNMR,^(31)P NMR,UV以及熔点测试等表征。

Carbonyldihydridotris（triphenylphosphine）ruthenium [RuH2 （CO）（Ph3P）3-] is one of the catalysts for catalytic addition in C--H bonds. It is prepared from trichlororuthenium, triphenylphosphines and formaldehyde in the presence of basic compounds. The effect of the quantity of triphenylphosphine, formaldehyde, solvent and the reaction time were studied. The optimal reaction conditions were found as follows： n（RuCl3· 3H2O） ： n（Ph3P） ： n（HCHO） ： n（KOH）= 1 ： 6 ： 160 ： 5.5, reaction time 2 h at 78 ℃. The yield of the product was above 84 %. The product was analyzed by IR, ^1H NMR, ^13C NMR, ^31p NMR, UV and melting point measurement.