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    • 2. 发明授权
    • Production of organophosphines
    • 生产有机膦
    • US4073810A
    • 1978-02-14
    • US549172
    • 1975-02-12
    • Klaus HestermannBernd LippsmeierGero Heymer
    • Klaus HestermannBernd LippsmeierGero Heymer
    • B01J21/00C07B61/00C07F9/50C07F9/53C07F9/54
    • C07F9/5086C07F9/54
    • Production of organophosphines of the general formula R.sub.n PH.sub.3-n, in which R stands for identical or different, substituted or unsubstituted alkyl, cycloalkyl or aralkyl groups having from 1 to 18 carbon atoms, preferably from 1 to 4 carbon atoms, more preferably from 1 to 2 carbon atoms, and n stands for a whole number within the range 1 and 3. The compounds are more particularly produced by continuously reacting hydrocarbon halides of the general formula RX, in which R has the meaning given hereinabove and X stands for halogen, especially for chlorine or bromine, with hydrogen phosphide, and primary or secondary organophosphines at temperatures within the range 100.degree. and 600.degree. C. and under pressures of up to 20 atmospheres in contact with a catalyst being placed in a reactor. Gaseous matter issuing from the reactor is cooled and the resulting organophosphonium halides (R.sub.n PH.sub.4-n)X are hydrolyzed in conventional manner to the corresponding organophosphines.
    • 制备通式RnPH3-n的有机膦,其中R代表相同或不同的取代或未取代的具有1至18个碳原子,优选1至4个碳原子的烷基,环烷基或芳烷基,更优选1至 2个碳原子,n表示1和3范围内的整数。化合物更特别地通过连续反应通式RX的卤代烃,其中R具有上文给出的含义,X代表卤素,特别是 对于氯或溴,与磷化氢以及初级或次级有机膦在100℃和600℃的温度范围内以及在与置于反应器中的催化剂接触的情况下在高达20个大气压的压力下进行。 将从反应器排出的气态物质冷却,并将所得的有机鏻卤化物(RnPH4-n)X以常规方式水解成相应的有机膦。
    • 4. 发明授权
    • Production of hydroxyalkylphosphine oxides
    • 生产羟烷基膦氧化物
    • US4076755A
    • 1978-02-28
    • US666699
    • 1976-03-15
    • Bernd LippsmeierKlaus Hestermann
    • Bernd LippsmeierKlaus Hestermann
    • C07F9/53C09K21/12
    • C09K21/12C07F9/5304
    • Production of tertiary hydroxyalkylphosphine oxides of general formula (I) ##STR1## in which R.sup.1 and R.sup.2 each stand for organic groups having from 1 to 18 carbon atoms, where R.sup.1 may be identical with R.sup.2 and R.sup.2 may be identical with R which stands for a radical of general formula (II) ##STR2## in which R.sup.3 and R.sup.4 equally stand for organic groups having from 1 to 18 carbon atoms and/or more preferably for hydrogen. The compounds are made from phosphines of general formula (III) ##STR3## in which R.sup.3 and R.sup.4 have the meanings given above, which are reacted in a single step operation with carbonyl compounds of general formula (IV) ##STR4## in which R.sup.3 and R.sup.4 equally have the meanings given above. The reaction is effected while adding at least one substance yielding hydroxyl ions and in the presence of water, and the resulting hydroxyalkylphosphine oxides are separated from the reaction product.
    • 其中R 1和R 2各自代表具有1至18个碳原子的有机基团,其中R 1可以与R 2和R 2相同,通式(Ⅰ)的叔羟烷基膦氧化物的制备可以与R相同, 代表通式(II)的基团(II),其中R 3和R 4均等于具有1至18个碳原子和/或更优选氢的有机基团。 化合物由通式(III)的膦制备,其中R 3和R 4具有上述含义,其在单步操作中与通式(IV)的羰基化合物(IMA)反应 IV),其中R3和R4同样具有上述含义。 在加入至少一种产生羟基离子的物质和水的存在下进行反应,并将所得羟烷基氧化膦与反应产物分离。
    • 5. 发明授权
    • Production of tertiary phosphine oxides
    • 生产叔膦氧化物
    • US4091012A
    • 1978-05-23
    • US780989
    • 1977-03-24
    • Hartfrid VollmerGeorg ElsnerBernd LippsmeierKlaus Hestermann
    • Hartfrid VollmerGeorg ElsnerBernd LippsmeierKlaus Hestermann
    • B01J27/00B01J31/00C07B61/00C07F9/53C07C120/00
    • C07F9/5304
    • Production of tertiary phosphine oxides which contain nitrile groups and correspond to the following general formula I: ##STR1## in which R.sup.1 and R.sub.2 each stand for a straight or branched, identical or different alkyl, cycloalkyl, aryl, alkylaryl or aralkyl group having 1 to 18 carbon atoms, and in which R.sup.1 or R.sub.2 may be identical with R, which stands for a radical of the following general formula II: ##STR2## in which R.sup.3 and R.sup.4 each stand for a straight or branched, identical or different alkyl, cycloalkyl, aryl, alkylaryl or aralkyl group having 1 to 18 carbon atoms, and/or hydrogen atoms. The tertiary phosphine oxides are made by reacting a phosphine of the following general formula III: ##STR3## in which R.sup.5 has the same meaning as R.sup.3 and R.sup.6 has the same meaning as R.sup.4 but is no hydrogen, with an .alpha.,.beta.-unsaturated nitrile of the following general formula IV: ##STR4## in which R.sup.3 and R.sup.4 have the meanings given above. The reaction is effected in a single stage in the presence of water or a water-solvent mixture and the above formula I compounds are separated from the reaction product.
    • 制备含有腈基并且对应于以下通式I的叔膦氧化物:其中R 1和R 2各自表示直链或支链,相同或不同的具有1个碳原子的烷基,环烷基,芳基,烷基芳基或芳烷基 至18个碳原子,其中R 1或R 2可以与R相同,其代表下列通式II的基团:其中R 3和R 4各自代表直链或支链,相同或不同的烷基 ,具有1至18个碳原子的环烷基,芳基,烷基芳基或芳烷基,和/或氢原子。 叔膦氧化物通过使下列通式III的膦:其中R 5具有与R 3相同的含义,R 6具有与R 4相同的含义,但不具有氢,具有α,β-不饱和的 腈,其中R 3和R 4具有上述含义。 反应在水或水 - 溶剂混合物存在下在单一阶段进行,并且上述式I化合物与反应产物分离。
    • 6. 发明授权
    • Production of tertiary phosphine oxides
    • 生产叔膦氧化物
    • US3997611A
    • 1976-12-14
    • US562222
    • 1975-03-26
    • Bernd LippsmeierKlaus HestermannHubert Neumaier
    • Bernd LippsmeierKlaus HestermannHubert Neumaier
    • C07F9/53C07F9/02
    • C07F9/53
    • Production of tertiary phosphine oxides of the general formula (I): ##STR1## in which the substituents R.sub.1 and R.sub.2, being identical or different, each stand for an alkyl, alkenyl, alkinyl, cycloalkyl, aralkyl or aryl radical having from 1 to 18 carbon atoms. The phosphine oxides are made by splitting off formaldehyde and hydrogen halide at temperatures within the range about 150.degree. and 350.degree. C, in the presence of hydrogen halide, from a molten compound of the general formula (II): ##STR2## in which R.sub.1 and R.sub.2 have the meanings given above and X stands for halogen; separating the formaldehyde and hydrogen split off from the reaction mixture, and treating the resulting crude product so as to separate the compound of general formula (I) therefrom.
    • 制备通式(I)的叔膦氧化物:其中取代基R 1和R 2相同或不同,各自代表具有烷基,烯基,炔基,环烷基,芳烷基或芳基,其具有 1至18个碳原子。 氧化膦通过在卤化氢存在下,在通式(II)的熔融化合物:分解甲醛和卤化氢的温度在约150℃和350℃的温度范围内制备。 其中R1和R2具有上述含义,X代表卤素; 分离从反应混合物中分离的甲醛和氢,并处理所得粗产物,以从其中分离出通式(I)的化合物。