Process for the preparation of chlorofluronitrobenzenes and
difluoronitrobenzenes
    231.
    发明授权
    Process for the preparation of chlorofluronitrobenzenes and difluoronitrobenzenes 失效
    氯氟草硝和二氟硝基苯的制备方法

    公开(公告)号:US5545768A

    公开(公告)日:1996-08-13

    申请号:US958107

    申请日:1992-12-22

    CPC classification number: C07C201/12

    Abstract: A process for the preparation of chlorofluoronitrobenzenes and difluoronitrobenzenes, which comprises heating dichloronitrobenzene to not more than 200.degree. C. in excess with an alkali metal fluoride having a total water content of about 0.2 to about 2.5% by weight in the presence of a quaternary ammonium and/or phosphonium salt, crown ether and/or polyethylene glycol dimethyl ether as catalyst in the absence of a solvent.

    Abstract translation: PCT No.PCT / EP92 / 01079 Sec。 371日期1992年12月22日 102(e)日期1992年12月22日PCT Filed 1991年6月8日PCT公布。 公开号WO91 / 00270 日期1992年1月9日一种氯氟硝基苯和二氟硝基苯的制备方法,其包括在二氯硝基苯与总含水量为约0.2至约2.5重量%的碱金属氟化物中将二氯硝基苯过量加热至不超过200℃ 在不存在溶剂的情况下存在季铵和/或鏻盐,冠醚和/或聚乙二醇二甲醚作为催化剂。

    Readily soluble, amorphous polyimide, and preparation process of same
    232.
    发明授权
    Readily soluble, amorphous polyimide, and preparation process of same 失效
    易溶,无定形聚酰亚胺及其制备方法相同

    公开(公告)号:US5480965A

    公开(公告)日:1996-01-02

    申请号:US280551

    申请日:1994-07-26

    Abstract: This invention relates to a novel thermoplastic and amorphous polyimide which is readily soluble in organic solvent, a novel aromatic diamino compound used for the polyimide, a preparation process thereof, a polyimide-based resin composition comprising the thermoplastic polyimide and a fibrous reinforcement, a process for preparing the resin composition, an injection molded article of the resin composition, a polyimide-based composite obtained by molding the above soluble and thermoplastic polyimide in combination with a fibrous reinforcement, and a fibrous reinforcement having a surface modified with the above polyimide.The polyimide comprise a requisite structural unit having one or more recurring structural units of the formula: ##STR1## wherein m and n are individually an integer of 0 or 1, and R is ##STR2## The polyimide of the invention is essentially amorphous, excellent in melt flow stability in the decreased temperature as compared with conventionally known polyimide and has greatly improved processability.The polyimide of the invention obtained by using a novel aromatic diamino compound as a monomer can control various properties such as melt flow ability and solubility in solvents by side chains and not by principal chain of polyimide. Thus, excellent melt flow property and solubility in solvents can be obtained while maintaining high heat resistance and adhesive property which are derived from benzophenone structure of the diamino compound of the the invention.

    Abstract translation: 本发明涉及易溶于有机溶剂的新型热塑性和无定形聚酰亚胺,用于聚酰亚胺的新型芳族二氨基化合物及其制备方法,包含热塑性聚酰亚胺和纤维增强剂的聚酰亚胺基树脂组合物, 用于制备树脂组合物的树脂组合物的注塑制品,通过将上述可溶性和热塑性聚酰亚胺与纤维增强剂组合成型而获得的聚酰亚胺类复合材料和具有用上述聚酰亚胺改性的表面的纤维增强剂。 聚酰亚胺包含必需的结构单元,其具有一个或多个下式的重复结构单元:其中m和n分别为0或1的整数,R为本发明的聚酰亚胺基本上为 与常规已知的聚酰亚胺相比,在降低的温度下的熔体流动稳定性优异并且具有极大的改进的加工性。 通过使用新颖的芳族二氨基化合物作为单体获得的本发明的聚酰亚胺可以通过侧链而不是聚酰亚胺的主链来控制各种性能如熔体流动性和在溶剂中的溶解度。 因此,在保持由本发明的二氨基化合物的二苯甲酮结构得到的高耐热性和粘合性的同时,可以获得优异的熔体流动性和溶剂中的溶解性。

    Synthesis of bis(2,2-dinitropropyl) formal (BDNPF)
    233.
    发明授权
    Synthesis of bis(2,2-dinitropropyl) formal (BDNPF) 失效
    双(2,2-二硝基丙基)正己烷(BDNPF)的合成

    公开(公告)号:US5449835A

    公开(公告)日:1995-09-12

    申请号:US339140

    申请日:1994-11-14

    CPC classification number: C07C201/12

    Abstract: A nonsolvent process of synthesizing bis(2,2-dinitropropyl)formal (BDNPF) is disclosed. In the process, 2,2-dinitropropanol (DNPOH) is reacted at low temperature with a formaldehyde source in the presence of a protic acid catalyst, such as H.sub.2 SO.sub.4, HCl, H.sub.3 PO.sub.4, or HBr. To inhibit byproduct formation, the reaction temperature is maintained from about -30.degree. C. to 30.degree. C. Upon completion of the reaction, the reaction solution is quenched with water and washed with an aqueous hydroxide ion solution. The hydroxide ion concentration should be sufficient to neutralize the protic acid catalyst during the quenching step and to solubilize unreacted 2,2-dinitropropanol as well as other aqueous soluble byproducts in the reaction solution. The BDNPF product is extracted with a low boiling temperature polar organic solvent, such as methyl tert-butyl ether (MTBE) or equivalent solvent. The organic solvent is evaporated to yield usable BDNPF product. The resulting yield is at least 60% based on the starting quantity of 2,2-dinitropropanol.

    Abstract translation: 公开了合成双(2,2-二硝基丙基)甲醛(BDNPF)的非溶剂方法。 在此过程中,在质子酸催化剂如H 2 SO 4,HCl,H 3 PO 4或HBr存在下,将2,2-二硝基丙醇(DNPOH)在低温下与甲醛源反应。 为了抑制副产物形成,将反应温度保持在约-30℃至30℃。反应完成后,将反应溶液用水淬灭并用氢氧化钠水溶液洗涤。 氢氧根离子浓度应足以在淬火步骤期间中和质子酸催化剂,并将未反应的2,2-二硝基丙醇以及其它水溶性副产物溶解在反应溶液中。 BDNPF产物用低沸点极性有机溶剂如甲基叔丁基醚(MTBE)或等效溶剂萃取。 将有机溶剂蒸发,得到可用的BDNPF产物。 基于2,2-二硝基丙醇的起始量,所得产率为至少60%。

    Process for the production of 5-alkoxy-2,4-dinitro-alkylbenzenes
    234.
    发明授权
    Process for the production of 5-alkoxy-2,4-dinitro-alkylbenzenes 失效
    5-烷氧基-2,4-二硝基 - 烷基苯的制备方法

    公开(公告)号:US5382702A

    公开(公告)日:1995-01-17

    申请号:US142383

    申请日:1993-11-19

    CPC classification number: C07C201/08 C07C201/12

    Abstract: Process for producing 5-alkoxy-2,4-dinitroalkylbenzenes of the general formula (I) ##STR1## R.sup.1 =C.sub.1 to C.sub.4 alkyl; R=C.sub.1 to C.sub.6 alkyl group, C.sub.2 to C.sub.4 hydroxyalkyl, C.sub.3 to C.sub.4 dihydroxyalkyl,in which a 3-fluoroalkylbenzene is nitrated and the obtained 2,4-dinitro-5-fluoroalkylbenzene is then reacted with a suitable alcohol at -5.degree. C. to +25.degree. C. with the addition of sodium hydroxide or potassium hydroxide.

    Abstract translation: PCT No.PCT / EP93 / 00678 Sec。 371日期:1993年11月19日 102(e)1993年11月19日PCT 1993年3月20日PCT PCT。 出版物WO93 / 2551200 日本1993年12月23日。通式(I)的5-烷氧基-2,4-二硝基烷基苯的制备方法(Ⅰ)R1 = C1〜C4烷基; R = C1至C6烷基,C2至C4羟基烷基,C3至C4二羟基烷基,其中3-氟烷基苯被硝化,所得2,4-二硝基-5-氟烷基苯然后与适当的醇在-5℃下反应 至+ 25℃,加入氢氧化钠或氢氧化钾。

    Process for preparing aromatic olefins
    235.
    发明授权
    Process for preparing aromatic olefins 失效
    芳烃烯烃的制备方法

    公开(公告)号:US5360924A

    公开(公告)日:1994-11-01

    申请号:US177945

    申请日:1994-01-06

    CPC classification number: C07C67/343

    Abstract: Process for preparing aromatic olefins of the formula (1) ##STR1## in which R.sup.1 -R.sup.3 are hydrogen, alkyl (C.sub.1 -C.sub.8) , alkoxy-(C.sub.1 -C.sub.5), phenyl, fluorine, chlorine, bromine, --OH, --NO.sub.2, --CN, --CHO, --COalkyl(C.sub.1 -C.sub.4) , --COphenyl, --COOalkyl (C.sub.1 -C.sub.4) , --OCOalkyl(C.sub.1 -C.sub.4), --NHCOalkyl(C.sub.1 -C.sub.4) , --CF.sub.3, --NH.sub.2, --NH--alkyl(C.sub.1 -C.sub.4) or --N(alkyl(C.sub.1 -C.sub.4)).sub.2 and R.sup.4 is hydrogen, alkyl(C.sub.1 -C.sub.8), phenyl, fluorine, chlorine, bromine, --OH, --NO.sub.2, --CN, --CHO or --OCOalkyl (C.sub.1 -C.sub.4) , and X is, inter alia, alkenyl(C.sub.2 -C.sub.12) or cycloalkenyl(C.sub.4 -C.sub.8) or the group ##STR2## in which R.sup.5 and R.sup.6 are, independently of one another, hydrogen or methyl, and Y is --phenyl, --CN, --COOH, --COOalkyl(C.sub.1 -C.sub.12), --COOphenyl, ##STR3## --CON (phenyl).sub.2, --COalkyl(C.sub.1 -C.sub.12), --COphenyl, --Oalkyl(C.sub.1 -C.sub.12) , --Ophenyl or the radical ##STR4## in which R.sup.1 -R.sup.4 are as defined above, by reacting an aryldiazonium salt of the formula (2) ##STR5## in which R.sup.1 -R.sup.4 are as defined and Z is the equivalent of an anion of an acid having a pK.sub.a of less than 7, with an olefin of the formula (3)HX (3)

    Abstract translation: 制备式(1)的芳族烯烃的方法其中R1-R3是氢,烷基(C1-C8),烷氧基 - (C1-C5),苯基,氟,氯,溴,-OH ,-NO 2,-CN,-CHO,-CO烷基(C1-C4),-CO苯基,-COO烷基(C1-C4),-OCO烷基(C1-C4),-NHCO烷基(C1-C4) ,-NH-烷基(C1-C4)或-N(烷基(C1-C4))2,R4是氢,烷基(C1-C8),苯基,氟,氯,溴,-OH,-NO2,-CN ,-CHO或-OCO烷基(C1-C4),X特别是链烯基(C2-C12)或环烯基(C4-C8)或其中R5和R6彼此独立的基团 氢或甲基,Y是 - 苯基,-CN,-COOH,-COO烷基(C1-C12),-COO苯基,-CON(苯基)2,-CO-烷基(C1-C12) (2)的芳基重氮盐(其中R1-R4如上所定义)的基团(C1-C12), - 苯基或其中R1-R4如上所定义的基团 Z是相当于pKa小于7的酸的阴离子与下式的烯烃 (3)HX(3)

    Aqueous synthesis of 2-halo-4,6-dinitroresorcinol and
4,6-diaminoresorcinol
    236.
    再颁专利
    Aqueous synthesis of 2-halo-4,6-dinitroresorcinol and 4,6-diaminoresorcinol 失效
    2-卤代-4,6-二硝基间苯二酚和4,6-二氨基间苯二酚的水合成

    公开(公告)号:USRE34589E

    公开(公告)日:1994-04-19

    申请号:US966663

    申请日:1992-10-26

    Inventor: Tyze-Kuan T. Yin

    CPC classification number: C07C201/12

    Abstract: The displacement of halogen from a 1,2,3-trihalo-4,6-dinitroresorcinol can be carried out in an aqueous medium using alkali metal hydroxide to form 2-halo-4,6-dinitroresorcinol. The product is a useful intermediate in the synthesis of 4,6-diaminoresorcinol, which is a monomer for polybenzoxazole polymers. The process from part of a useful aqueous process for synthesizing 4,6-diaminoresorcinol.

    Abstract translation: 卤素从1,2,3-三卤代-4,6-二硝基间苯二酚的位移可以在含水介质中使用碱金属氢氧化物进行,形成2-卤代-4,6-二硝基间苯二酚。 该产物是合成4,6-二氨基间苯二酚的有用中间体,它是聚苯并恶唑聚合物的单体。 用于合成4,6-二氨基间苯二酚的部分有用的水性方法的方法。

    Preparation of bis(3-nitrophenoxy) compound
    237.
    发明授权
    Preparation of bis(3-nitrophenoxy) compound 失效
    双(3-硝基苯氧基)化合物的制备

    公开(公告)号:US5296635A

    公开(公告)日:1994-03-22

    申请号:US975952

    申请日:1992-11-13

    CPC classification number: C07C201/12 C07C315/04 C07C319/20

    Abstract: A preparation process of a bis(3-nitrophenoxy) compound represented by the formula: ##STR1## wherein X is a direct bond, divalent hydrocarbon having from 1 to 10 carbon atoms or a divalent group selected from --C(CF.sub.3).sub.2, --CO--, --S--, --SO--, SO.sub.2 --or --O--, which comprises reacting 4,4'-bisphenol with m-dinitrobenzene in the presence of an alkali metal carbonate or alkali metal hydrogen carbonate having a particle size of 250 .mu.m or less while removing generated water from the reaction system during the reaction. In one embodiment of the process, the reaction is carried out while simultaneously adding 4,4'-bisphenol and m-dinitrobenzene to a reaction vessel which was previously charged with the base and an aprotic polar solvent.

    Abstract translation: 由下式表示的双(3-硝基苯氧基)化合物的制备方法:其中X是直接键,具有1至10个碳原子的二价烃或选自-C(CF 3)2 - 的二价基团, CO-,-S-,-SO-,SO 2 - 或-O-,其包括在碱金属碳酸盐或粒度为250的碱金属碳酸氢盐存在下使4,4'-双酚与间二硝基苯反应 在反应期间从反应体系中除去产生的水。 在该方法的一个实施方案中,反应进行同时向预先装入碱和反质子极性溶剂的反应容器中加入4,4'-双酚和间二硝基苯。

    4-hydroxy-2'-nitrobutyrophenone and
tetrahydro-2-(o-nitrophenyl)-2-furanol useful as intermediates in the
preparation of a crop-selective herbicide
    239.
    发明授权
    4-hydroxy-2'-nitrobutyrophenone and tetrahydro-2-(o-nitrophenyl)-2-furanol useful as intermediates in the preparation of a crop-selective herbicide 失效
    4-羟基-2'-硝基苯丙酮和四氢-2-(邻硝基苯基)-2-呋喃醇可用作制备作物选择性除草剂的中间体

    公开(公告)号:US5281726A

    公开(公告)日:1994-01-25

    申请号:US997844

    申请日:1992-12-29

    Inventor: David A. Cortes

    CPC classification number: C07D307/20 C07C205/45

    Abstract: There are provided 4-Hydroxy-2'-nitrobutyrophenone and tetrahydro-2-(o-nitrophenyl)-2-furanol and mixtures thereof, important intermediates in the preparation of the crop-selective herbicidal agent 1-{[o-(cyclopropylcarbonyl)phenyl]sulfamoyl}-3-(4,6-dimethoxy-2-pyrimidinyl)urea. Also provided is a method for the preparation of 4-halo-2'-nitrobutyrophenone, useful as an intermediate in the preparation of 1-{[o-(cyclopropylcarbonyl)phenyl]sulfamoyl}-3-(4,6-dimethoxy-2-pyrimidinyl)urea.

    Abstract translation: 提供4-羟基-2'-硝基苯丙酮和四氢-2-(邻硝基苯基)-2-呋喃醇及其混合物,其是制备作物选择性除草剂1 - ((邻 - (环丙基羰基) 苯基)氨磺酰)-3-(4,6-二甲氧基-2-嘧啶基)脲。 还提供了制备4-卤代-2'-硝基苯丙酮的方法,其可用作制备1 - ((邻 - (环丙基羰基)苯基)氨磺酰基)-3-(4,6-二甲氧基-2 - 嘧啶基)脲。

    Monofunctionalization of phenolic hydroxy onto a polyphenol
    240.
    发明授权
    Monofunctionalization of phenolic hydroxy onto a polyphenol 失效
    苯酚羟基在聚苯酚上的单官能化

    公开(公告)号:US5198571A

    公开(公告)日:1993-03-30

    申请号:US807982

    申请日:1991-12-16

    Abstract: A region-specific monofunctionalization of a phenolic hydroxy onto a polyphenol for the preparation of a compound of the formula ##STR1## wherein R is selected from the group consisting of hydrogen, alkyl of 1 to 8 carbon atoms, alkenyl and alkynyl of 2 to 8 carbon atoms, --CN, formyl, carboxy, alkoxy carbonyl of up to 9 carbon atoms, aralkoxy carbonyl or up to 12 carbon atoms and halogen and R' is a hydroxy protective group comprising reacting a polyphenol of the formula ##STR2## wherein R has the above definition with a base to form the corresponding dianion, reacting the latter with a trialkyl borate of the formulaB(OAlk).sub.3wherein Alk is alkyl of 1 to 6 carbon atoms to form a compound of the formula ##STR3## reacting the latter with a reagent capable of introducing a hydroxy protective group and reacting the latter with a hydrolysis agent for the oxygen-boron bond to obtain the corresponding compound of Formula I.

    Abstract translation: 苯酚羟基对多酚的区域特异性单官能化,用于制备下式化合物其中R选自氢,1至8个碳原子的烷基,2至2的烯基和炔基 8个碳原子,-CN,甲酰基,羧基,至多9个碳原子的烷氧基羰基,芳烷氧基羰基或至多12个碳原子和卤素,R'是羟基保护基,包括使式II的多酚反应其中 R具有上述定义与碱形成相应的二价阴离子,使后者与式B的三烷基硼酸盐(OAlk)3反应,其中Alk是1至6个碳原子的烷基,以形成式III的化合物 使后者与能够引入羟基保护基的试剂反应,并将其与用于氧 - 硼键的水解剂反应,得到相应的式I化合物。

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