申请人:STAUFFER CHEMICAL COMPANY
公开号:EP0196742A1
公开(公告)日:1986-10-08
A process is disclosed for preparing alkyldiarylphosphines and related compounds. In such process a compound having the structural formula:
wherein :
Z is an atom from group VA of the periodic table;
Y is any radical that is essentially incapable of reacting with an alkali metal;
X is any radical that is essentially incapable of reacting with an alkali metal;
W is a substituted or unsubstituted aryl, alkyl, arylalkyl, or alkylaryl radical or hydrogen; and
is prepared by reacting a first halide with a molten alkali metal or amalgam thereof in the presence of an inert solvent to form a first reacted mixture which is reacted with a second halide wherein an amount of the alkali metal or amalgam thereof is used in an excess of less than 100% and the yield of the product is greater than 70%. Typically, diphenylphosphinous chloride is reacted in solution with an excess of an alkali metal; and the reaction product reacted with chorohex- ane thereby forming hexyldiphenylphosphine. The improved process produces greater yields, by use of critical amounts of alkali metal; use of a single reactor rather than two reactors; preinitiation of the first stage reaction reduction of temperatures to increase reaction rate under certain conditions; and preferred reactants and physical form thereof. Novel products include behenyldiphenylphosphine.
本发明公开了一种制备烷基叔基膦及相关化合物的工艺。在该工艺中,化合物的结构式为
其中:
Z 是元素周期表 VA 族中的原子;
Y 是基本上不能与碱金属反应的任何基团;
X 是基本上不能与碱金属反应的任何基团;
W 是取代或未取代的芳基、烷基、芳烷基或烷芳基或氢;以及
制备方法是:在惰性溶剂存在下,使第一种卤化物与熔融碱金属或其汞齐反应,形成第一种反应混合物,该混合物与第二种卤化物反应,其中碱金属或其汞齐的使用过量小于 100%,产物的收率大于 70%。通常,二苯基氯化膦在溶液中与过量的碱金属反应,反应产物与氯己烯反应,从而形成羟基二苯基膦。改进后的工艺产量更高,因为它使用了临界量的碱金属;使用了单个反应器而不是两个反应器;预引发了第一阶段反应,降低了温度以提高特定条件下的反应速率;以及优选的反应物及其物理形式。新产品包括苯基二苯基膦。