Method for preparing 2,3-dimethyl-2,3-dinitrobutane
    35.
    发明授权
    Method for preparing 2,3-dimethyl-2,3-dinitrobutane 有权
    制备2,3-二甲基-2,3-二硝基丁烷的方法

    公开(公告)号:US08692036B2

    公开(公告)日:2014-04-08

    申请号:US13823831

    申请日:2011-09-05

    CPC classification number: C07C201/14 C07C201/06 C07C205/02

    Abstract: The present invention relates to a method for preparing 2,3-dimethyl-2,3-dinitrobutane (DMNB), which includes the following steps: (1) making titanium-silicate molecular sieve catalyst, acetone, hydrogen peroxide and ammonia contact and react at 65-80° C. to obtain a modified titanium-silicate molecular sieve catalyst; and (2-1) making acetone oxime and hydrogen peroxide contact and react in the presence of the modified titanium-silicate molecular sieve catalyst and water under the conditions of temperature of 60-90° C. and pH of 8-10, and separating DMNB from the reaction products thereof; or (2-2) making acetone, ammonia and hydrogen peroxide contact and react in the presence of the modified titanium-silicate molecular sieve catalyst and water under the conditions of temperature of 60-90° C. and pH of 8-10, and separating DMNB from the reaction products thereof. By the method provided by the present invention, DMNB can be prepared without having to use dangerous chemicals, such as 2-nitropropane, NaH and the like.

    Abstract translation: 本发明涉及一种制备2,3-二甲基-2,3-二硝基丁烷(DMNB)的方法,其包括以下步骤:(1)使钛硅酸盐分子筛催化剂,丙酮,过氧化氢和氨接触并反应 在65-80℃下,得到改性钛酸酯分子筛催化剂; 和(2-1)使丙酮肟和过氧化氢接触并在改性的钛酸硅酸盐分子筛催化剂和水的存在下在60-90℃的温度和pH为8-10的条件下反应,并分离 DMNB反应产物; 或(2-2)使丙酮,氨和过氧化氢接触并在改性钛硅酸盐分子筛催化剂和水的存在下在60-90℃的温度和pH为8-10的条件下反应,和 从其反应产物中分离DMNB。 通过本发明提供的方法,可以制备DMNB,而不必使用危险化学品,例如2-硝基丙烷,NaH等。

    Method for producing dinitrotoluene
    36.
    发明授权
    Method for producing dinitrotoluene 有权
    二硝基甲苯生产方法

    公开(公告)号:US07851661B2

    公开(公告)日:2010-12-14

    申请号:US10586683

    申请日:2005-02-02

    CPC classification number: C07C201/08 C07C201/14 C07C205/06

    Abstract: The present invention provides a process for preparing dinitrotoluene, comprising the steps of a) reacting toluene with nitric acid in the presence of sulphuric acid to give mononitrotoluene, b) separating the reaction product from step a) into an organic phase comprising mononitrotoluene and an aqueous phase comprising sulfuric acid, c) reacting the organic phase comprising mononitrotoluene with nitric acid in the presence of sulphuric acid to give dinitrotoluene, d) separating the reaction product from step c) into an organic phase comprising dinitrotoluene and an aqueous phase comprising sulfuric acid, wherein the reaction product from step a) has a content of toluene of from 3.0 to 8% by weight, based on the organic phase, and a content of nitric acid of from 0.1 to 1.2% by weight, based on the aqueous phase, and the phase separation in step b) is effected in such a way that further reaction of the toluene with the nitric acid is prevented.

    Abstract translation: 本发明提供了制备二硝基甲苯的方法,包括以下步骤:a)在硫酸存在下使甲苯与硝酸反应得到一硝基甲苯,b)将步骤a)中的反应产物分离成包含单硝基甲苯和水 相,包括硫酸,c)在硫酸存在下使包含一硝基甲苯的有机相与硝酸反应,得到二硝基甲苯,d)将步骤c)中的反应产物分离成包含二硝基甲苯和含有硫酸的水相的有机相, 其中步骤a)的反应产物的甲苯含量为3.0-8重量%,基于有机相,硝酸含量为0.1-1.2重量%,基于水相,和 步骤b)中的相分离是以防止甲苯与硝酸进一步反应的方式进行的。

    Substituted 1,1,1-triaryl-2,2,2-trifluoroethanes and processes for their
synthesis
    38.
    发明授权
    Substituted 1,1,1-triaryl-2,2,2-trifluoroethanes and processes for their synthesis 失效
    取代的1,1,1-三芳基-2,2,2-三氟乙烷及其合成方法

    公开(公告)号:US4912238A

    公开(公告)日:1990-03-27

    申请号:US292049

    申请日:1988-12-30

    Abstract: Synthetic procedures to tetraalkyls, tetraacids and dianhydrides substituted 1,1,1-triaryl-2,2,2-trifluoroethanes which comprises: (1) 1,1-bis(dialkylaryl)-1-aryl-2,2,2-trifluoroethane, (2) 1,1-bis(dicarboxyaryl)-1-aryl-2,2,2-trifluoroethane or (3) cyclic dianhydride or diamine of 1,1-bis(dialkylaryl)-1-aryl-2,2,2-trifluoroethanes. The synthesis of (1) is accomplished by the condensation reaction of an aryltrifluoromethyl ketone with a dialkylaryl compound. The synthesis of (2) is accomplished by oxidation of (1). The synthesis dianhydride of (3) is accomplished by the conversion of (2) to its corresponding cyclic dianhydride. The synthesis of the diamine is accomplished by the similar reaction of an aryltrifluoromethyl ketone with aniline or alkyl substituted or disubstituted anilines. Also, other derivatives of the above are formed by nucleophilic displacement reactions.

    Abstract translation: 四烷基,四酸和二酐的合成方法取代1,1,1-三芳基-2,2,2-三氟乙烷,其包括:(1)1,1-双(二烷基芳基)-1-芳基-2,2,2-三氟乙烷 ,(2)1,1-双(二羧基芳基)-1-芳基-2,2,2-三氟乙烷或(3)1,1-双(二烷基芳基)-1-芳基-2,2,2-三氟乙烷的环状二酐或二胺, 2-三氟乙烷。 (1)的合成通过芳基三氟甲基酮与二烷基芳基化合物的缩合反应来实现。 (2)的合成通过(1)的氧化实现。 (3)的合成二酐通过(2)转化成其相应的环状二酐来实现。 二胺的合成通过芳基三氟甲基酮与苯胺或烷基取代或二取代的苯胺的类似反应来实现。 此外,上述的其它衍生物通过亲核取代反应形成。

    Substituted 1,1,1-triaryl-2,2,2-trifluoroethanes and processes for their
synthesis
    39.
    发明授权
    Substituted 1,1,1-triaryl-2,2,2-trifluoroethanes and processes for their synthesis 失效
    取代的1,1,1-三芳基-2,2,2-三氟乙烷及其合成方法

    公开(公告)号:US4885116A

    公开(公告)日:1989-12-05

    申请号:US159071

    申请日:1988-02-23

    Abstract: Synthetic procedures to tetraalkyls, tetraacids and dianhydrides substituted 1,1,1-triaryl-2,2,2-trifluoroethanes which comprises: (1) 1,1-bis(dialkylaryl)-1-aryl-2,2,2-trifluoroethane, (2) 1,1-bis(dicarboxyaryl)-1-aryl-2,2,2-trifluoroethane or (3) cyclic dianhydride or diamine of 1,1-bis(dialkylaryl)-1-aryl-2,2,2-trifluoroethanes. The synthesis of (1) is accomplished by the condensation reaction of an aryltrifluoromethyl ketone with a dialkylaryl compound. The synthesis of (2) is accomplished by oxidation of (1). The synthesis dianhydride of (3) is accomplished by the conversion of (2) to its corresponding cyclic dianhydride. The synthesis of the diamine is accomplished by the similar reaction of an aryltrifluoromethyl ketone with aniline or alkyl substituted or disubstituted anilines. Also, other derivatives of the above are formed by nucleophilic displacement reactions.

    Abstract translation: 四烷基,四酸和二酐的合成方法取代1,1,1-三芳基-2,2,2-三氟乙烷,其包括:(1)1,1-双(二烷基芳基)-1-芳基-2,2,2-三氟乙烷 ,(2)1,1-双(二羧基芳基)-1-芳基-2,2,2-三氟乙烷或(3)1,1-双(二烷基芳基)-1-芳基-2,2,2-三氟乙烷的环状二酐或二胺, 2-三氟乙烷。 (1)的合成通过芳基三氟甲基酮与二烷基芳基化合物的缩合反应来实现。 (2)的合成通过(1)的氧化实现。 (3)的合成二酐通过(2)转化成其相应的环状二酐来实现。 二胺的合成通过芳基三氟甲基酮与苯胺或烷基取代或二取代的苯胺的类似反应来实现。 此外,上述的其它衍生物通过亲核取代反应形成。

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