公开(公告)号：EP0196742A1

公开(公告)日：1986-10-08

申请号：EP86300592.2

申请日：1986-01-29

Applicant: STAUFFER CHEMICAL COMPANY

Inventor： Bay, William Elliott ,  Reineke, Karl Edward ,  Weil, Edward David

IPC: C07F9/50

CPC classification number: C07F9/5077

Abstract: 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.

Abstract translation: 公开了制备烷基二芳基膦和相关化合物的方法。 在这种方法中，具有以下结构式的化合物：其中：Z是周期表第VA族的原子; Y是基本上不能与碱金属反应的任何基团; X是任何 基本上不能与碱金属反应的基团; W是取代或未取代的芳基，烷基，芳基烷基或烷基芳基或氢; 和... U是氢或... ...或卤素; ...通过使第一卤化物与熔融碱金属或汞齐在惰性溶剂的存在下反应以形成与第二卤化物反应的第一反应混合物 其中使用的碱金属或汞的量超过100％，产物的收率大于70％。 通常，二苯基次氯化物在溶液中与过量的碱金属反应; 反应产物与己烷反应，从而形成己基二苯基膦。 改进的方法通过使用临界量的碱金属产生更高的产率; 使用单个反应器而不是两个反应器; 在某些条件下第一阶段反应降低温度以提高反应速率; 和优选的反应物及其物理形式。 新产品包括二苯基二苯基膦。

公开(公告)号：EP0251246A1

公开(公告)日：1988-01-07

申请号：EP87109226.8

申请日：1987-06-26

Applicant: STAUFFER CHEMICAL COMPANY

Inventor： Leone-Bay, Andrea ,  Bay, William Elliott ,  Timony, Peter Edward

IPC: C07B39/00 ,  C07F9/535

CPC classification number: C07F9/535 ,  C07B39/00 ,  C07C17/16 ,  C07D213/61 ,  C07C22/00

Abstract: A process for converting organic hydroxyl-containing compounds to halides which comprises reacting the hydroxyl-­containing compound with a phosphorushalide reagent of formula: R n PX 5-n wherein n is selected from 1, 2 and 3; R is selected from the group consisting of C-6 to C-10 aryl and substituted aryl wherein the substituents are selected from the group consisting of straight and branched chain alkyl, alkoxy, and haloalkyl, halogen, sulfonate and mixtures thereof; and X is a halogen. It is preferred to carry out the reaction in the presence of an arylphosphorus­oxydihalide solvent. The use of an arylphosphorustetra­halide and particularly phenylphosphorustetrachloride is preferred. The arylphosphorustetrahalide can be prepared in situ by contacting a solution of the corresponding arylphosphorusdihalide in an arylphosphorusoxydihalide solvent with a halogen. The process can further comprise the step of heating the reaction mixture. Maintaining a reaction temperature of from about 0°C to about 150°C for from about 1 hour to about 24 hours is preferred.

Abstract translation: 一种将有机含羟基化合物转化为卤化物的方法，包括使含羟基化合物与式RnPX5-n的磷酸盐试剂反应，其中n选自1,2和3; R选自C-6至C-10芳基和取代的芳基，其中取代基选自直链和支链烷基，烷氧基和卤代烷基，卤素，磺酸酯及其混合物; X为卤素。 优选在芳基磷酸二卤化物溶剂存在下进行反应。 使用芳基磷酰四卤化物，特别是苯基四氯化锡是优选的。 芳基次磷酸四卤化物可以通过将相应的芳基二卤代二芳基磷酸二卤化物溶剂中的溶液与卤素接触来原位制备。 该方法还可以包括加热反应混合物的步骤。 保持约0℃至约150℃的反应温度约1小时至约24小时是优选的。

公开(公告)号：EP0194716A1

公开(公告)日：1986-09-17

申请号：EP86200333.2

申请日：1986-03-03

Applicant: STAUFFER CHEMICAL COMPANY

Inventor： Bay, William Elliott ,  Reineke, Karl Edward

IPC: C07F9/50 ,  C07F9/53

CPC classification number: C07F9/53 ,  C07F9/5059

Abstract: There is disclosed an improved process for the addition of phospinesto alpha-olefins at high yields and conversions. The process involves the absence of a catalyst whose residues could interfere with the utility of the product, such as n-hexyldiphenylphosphine, as a ligand. Simple thermal reaction is used at temperatures of at least 200°C., most preferably 250°C - 350°C. The pressure is preferably at least atmospheric. Preferred reactants, pnoducts, and pracessing conditions are also disclosed. Batch processes are exemplified and continuous processes proposed.