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    • 1. 发明授权
    • Highly pure monoalkylphosphine and method for producing same
    • 高纯度单烷基膦及其制备方法
    • US6025525A
    • 2000-02-15
    • US216917
    • 1998-12-21
    • Masashi SugiyaTsutomu WatanabeNatsuhiro Sano
    • Masashi SugiyaTsutomu WatanabeNatsuhiro Sano
    • C07F9/50C07F9/28
    • C07F9/5004C07F9/5059C07F9/5095
    • A highly pure monoalkylphosphine which is useful as a starting material for producing a compound semiconductor, and a method for producing same in high yield are provided. The highly pure monoalkylphosphine is represented by the general formula RPH.sub.2 (wherein R is an alkyl group having 1 to 8 carbon atoms), has a purity of not less than 99.999%, and is substantially free of sulfur and silica. In the method of producing said highly pure monoalkylphosphine, anhydrous hydrofluoric acid is used as a catalyst for a reaction between phosphine and an alkene, and the reaction is carried out in the presence of an organic solvent having a boiling point higher than that of the resulting monoalkylphosphine; the resulting reaction mixture is contacted with an alkali solution so that the remaining catalyst is removed into an aqueous phase in the form of a fluoride salt; next, the obtained reaction mixture is contacted with an alkali hydride and the impurities are removed, then distillation is carried out.
    • 提供了可用作制备化合物半导体的起始材料的高纯度单烷基膦及其高产率制备方法。 高纯度单烷基膦由通式RPH 2(其中R是具有1至8个碳原子的烷基)表示,纯度不低于99.999%,并且基本上不含硫和二氧化硅。 在制造高纯度单烷基膦的方法中,使用无水氢氟酸作为膦与烯烃反应的催化剂,反应在沸点高于所得到的有机溶剂的存在下进行 单烷基膦; 将所得反应混合物与碱溶液接触,使剩余的催化剂以氟化物盐的形式除去到水相中; 接着,将得到的反应混合物与碱金属氢化物接触,除去杂质,然后进行蒸馏。
    • 2. 发明授权
    • Highly pure monoalkylphosphine and method for producing same
    • 高纯度单烷基膦及其制备方法
    • US5892120A
    • 1999-04-06
    • US977807
    • 1997-11-25
    • Masashi SugiyaTsutomu WatanabeNatsuhiro Sano
    • Masashi SugiyaTsutomu WatanabeNatsuhiro Sano
    • C07F9/50C07F9/52
    • C07F9/5004C07F9/5059C07F9/5095
    • A highly pure monoalkylphosphine which is useful as a starting material for producing a compound semiconductor, and a method for producing same in high yield are provided. A highly pure monoalkylphosphine represented by the general formula RPH.sub.2 (wherein R is an alkyl group having 1 to 8 carbon atoms) has a purity of not less than five nines, and is substantially free of sulfur and silica. In the method of producing said highly pure monoalkylphosphine, anhydrous hydrofluoric acid is used as a catalyst for a reaction between phosphine and an alkene, and the reaction is carried out in the presence of an organic solvent having a boiling point higher than that of the resulting monoalkylphosphine; the resulting reaction mixture is contacted with an alkali solution so that the remaining catalyst is removed into an aqueous phase in the form of a fluoride salt; next, the obtained reaction mixture is contacted with an alkali hydride and the impurities are removed, then distillation is carried out.
    • 提供了可用作制备化合物半导体的起始材料的高纯度单烷基膦及其高产率制备方法。 由通式RPH2(其中R是具有1至8个碳原子的烷基)表示的高纯度单烷基膦的纯度不低于5个,并且基本上不含硫和二氧化硅。 在制造高纯度单烷基膦的方法中,使用无水氢氟酸作为膦与烯烃反应的催化剂,反应在沸点高于所得到的有机溶剂的存在下进行 单烷基膦; 将所得反应混合物与碱溶液接触,使剩余的催化剂以氟化物盐的形式除去到水相中; 接着,将得到的反应混合物与碱金属氢化物接触,除去杂质,然后进行蒸馏。
    • 3. 发明授权
    • Process for preparing a phosphonium salt compound having an acryl group
    • 制备具有丙烯酰基的鏻盐化合物的方法
    • US6080885A
    • 2000-06-27
    • US153083
    • 1998-09-15
    • Masashi SugiyaTsutomu Watanabe
    • Masashi SugiyaTsutomu Watanabe
    • C07F9/54C07C69/52C07F9/02
    • C07F9/5407
    • A phosphonium salt compound having an acryl group which is represented by the following general formula (3) can be made in simple operations: ##STR1## (wherein A represents a alkylene group, Y represents Cl, Br or I, R.sup.1 represents H or CH.sub.3, and R.sup.2, R.sup.3 and R.sup.4 represent a alkyl group having 1-8 carbon atoms, cycloalkyl, aryl, alkaryl or aralkyl group) by reacting an unsaturated aliphatic carboxylic acid halide of the following general formula (1):CH.sub.2 .dbd.CR.sup.1 --COX (1)(wherein R.sup.1 represents H or CH.sub.3 and X represents Cl, Br or I) with a hydroxyalkyl phosphonium salt compound of the following general formula (2):[HO--A--P.sup.+ R.sup.2 R.sup.3 R.sup.4 ]Y.sup.- (2)(wherein A, Y, R.sup.2, R.sup.3 and R.sup.4 have the same meanings as defined above). The present invention is industrially advantageous since the product can have a very high purity and be obtained in high yield by an easy operation.
    • 具有以下通式(3)表示的具有丙烯酰基的鏻盐化合物可以简单地进行:(其中A表示亚烷基,Y表示Cl,Br或I,R1表示H或CH3,R2表示 通过使下列通式(1)的不饱和脂族羧酸卤化物:CH2 = CR1-COX(1)(其中,R3和R4表示具有1-8个碳原子的烷基,环烷基,芳基,烷芳基或芳烷基) 其中R1表示H或CH3,X表示Cl,Br或I)与下列通式(2)的羟烷基鏻盐化合物:[HO-A-P + R2R3R4] Y-(2)(其中A,Y, R2,R3和R4具有与上述相同的含义)。 本发明在工业上是有利的,因为产品可以具有非常高的纯度,并且通过容易的操作可以高产率获得。