Process for the preparation of sulfonic acid chlorides
    32.
    发明授权
    Process for the preparation of sulfonic acid chlorides 失效
    制备磺酸氯化物的方法

    公开(公告)号:US4166070A

    公开(公告)日:1979-08-28

    申请号:US817456

    申请日:1977-07-19

    申请人: Heinz U. Blank

    发明人: Heinz U. Blank

    摘要: A process for the preparation of a sulfonic acid chloride of the formula ##STR1## wherein R.sup.1, R.sup.2 and R.sup.3 are identical or different and denote hydrogen, a lower alkyl or cycloalkyl radical, halogen, aryl, aralkyl, aryl-ether or one of the radicals ##STR2## or where ADJACENT RADICALS R.sup.1 and R.sup.2 are linked to form a cycloaliphatic or aromatic carbocyclic ring which is optionally substituted by a sulfonic acid chloride groupWhich comprises contacting an aromatic compound of the formula ##STR3## wherein R.sup.1, R.sup.2 and R.sup.3 have the previously assigned significanceWith an approximately equimolar amount of a sulfonating agent, based upon the number of sulfonic acid chloride groups to be introduced and an excess of thionyl chloride, the sulfonating agent and thionyl chloride being initially introduced or added simultaneously with the addition of said aromatic compound.

    Process for the preparation of cyclopropanecarboxamide
    33.
    发明授权
    Process for the preparation of cyclopropanecarboxamide 失效
    制备环磷酰胺酰胺的方法

    公开(公告)号:US5068428A

    公开(公告)日:1991-11-26

    申请号:US588251

    申请日:1990-09-26

    CPC分类号: C07C231/02 C07C2101/02

    摘要: Cyclopropanecarboxamide can be prepared by reaction of a cyclopropanecarboxylic ester with NH.sub.3, in which the ester alcohol has 4-8 C atoms and can be straight-chain or branched and which process is carried out in the presence of catalytic amounts of an alkali metal alcoholate of a monohydric C.sub.1-C.sub.8 alcohol at 60.degree.-200.degree. C. in the absence of a hydrocarbon solvent.

    摘要翻译: 环丙烷甲酰胺可以通过环丙烷羧酸酯与NH 3反应来制备,其中酯醇具有4-8个C原子,并且可以是直链或支链的,该方法是在催化量的碱金属醇化物存在下进行的 在不存在烃溶剂的情况下,在60℃-200℃下加入一元醇C 1 -C 8醇。

    Process for the preparation of .mu.-amino-acrylic acid esters
    34.
    发明授权
    Process for the preparation of .mu.-amino-acrylic acid esters 失效
    制备μ-氨基 - 丙烯酸酯的方法

    公开(公告)号:US5030747A

    公开(公告)日:1991-07-09

    申请号:US495522

    申请日:1990-03-19

    CPC分类号: C07C227/06

    摘要: .beta.-Amino-acrylic acid esters of the formula(R.sup.1 R.sup.2)NCH.dbd.CR.sup.3 --COOR.sup.4can be obtained by reaction of .beta.-hydroxy-acrylic acid ester alkali metal salts of the formulaMe.sup..sym. .crclbar. OCH.dbd.CR.sup.3 --COOR.sup.4with ammonium salts of the formula(R.sup.1 R.sup.2) NH.sub.2.sup..sym. .crclbar.according to the general reaction equation(R.sup.1 R.sup.2) NH.sub.2 X+MeOCH.dbd.CR.sup.3 --COOR.sup.4 .fwdarw.(R.sup.1 R.sup.2) NCH.dbd.CR.sup.3 --COOR.sup.4 +MeX.dbd.H.sub.2 OR.sup.1, R.sup.2, R.sup.3, R.sup.4, Me.sup..sym. and X.sup..crclbar. having the meaning indicated in the description and the reaction being carried out in an aprotic organic solvent, in which the reaction components are suspended, as the reaction medium and it being possible to replace a part of the aprotic organic solvent by a protic organic solvent which is miscible with the aprotic solvent to give a homogeneous phase.

    摘要翻译: 式(R1R2)NCH = CR3-COOR4的β-氨基 - 丙烯酸酯可以通过将式Me(+)( - )OCH = CR 3 -COOR 4的β-羟基 - 丙烯酸酯碱金属盐与 (R1R2)NH2X + MeOCH = CR3-COOR4 - (R1R2)NCH = CR3-COOR4 + MeX = H2O R1,R2,R3的式(R1R2)NH2(+)( - )的铵盐 ,R4,Me(+)和X( - ),并且反应在其中悬浮反应组分的非质子有机溶剂中作为反应介质进行,并且可以代替 质子有机溶剂是非质子有机溶剂的一部分,其与非质子溶剂混溶以产生均相。

    Process for the preparation of 1,5-dihydroxynaphthalene and
1,5-diaminonaphthalene
    35.
    发明授权
    Process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene 失效
    制备1,5-二羟基萘和1,5-二氨基萘的方法

    公开(公告)号:US4973758A

    公开(公告)日:1990-11-27

    申请号:US439757

    申请日:1989-11-21

    摘要: The characteristic of the improved process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene is to carry out the alkaline pressure hydrolysis of the disodium salt of naphthalene-1,5-disulphonic acid at temperatures from 270.degree. to 290.degree. C. and under 14 to 20 bar using an excess of sodium hydroxide solution such that the molar ratio NaOH/disodium salt of naphthalenesulphonic acid is at least 12:1. The 1,5-dihydroxynaphthalene which is obtained in this manner, without hazard and in substantially higher purity, is then aminated with ammonia in the presence of ammonium bisulphite to give 1,5-diaminonaphthalene, it being possible to achieve a further increase in the degree of purity of the 1,5-diaminonaphthalene by increasing the molar ratio NH.sub.3 /1,5-dihydroxynaphthalene to at least 6:1.

    摘要翻译: 制备1,5-二羟基萘和1,5-二氨基萘的改进方法的特点是在270〜290℃的温度下进行萘-1,5-二磺酸二钠盐的碱性水解 并使用过量的氢氧化钠溶液使14至20巴,使得萘磺酸的NaOH /二钠盐的摩尔比至少为12:1。 然后用亚硫酸铵存在下用氨将胺化得到的1,5-二羟基萘没有危害并且纯度高得多,得到1,5-二氨基萘,可以进一步增加 通过将NH 3 / 1,5-二羟基萘的摩尔比提高到至少6:1,1,5-二氨基萘的纯度。

    Process for preparing p-toluidine-2-sulphonic acid
    38.
    发明授权
    Process for preparing p-toluidine-2-sulphonic acid 失效
    对甲苯胺-2-磺酸的制备方法

    公开(公告)号:US4717514A

    公开(公告)日:1988-01-05

    申请号:US848357

    申请日:1986-04-04

    CPC分类号: C07C309/45

    摘要: P-Toluidine-2-sulphonic acid (5-amino-2-methylbenzenesulphonic acid) is obtained in very pure form and virtually free of p-toluidine-3-sulphonic acid (2-amino-5-methylbenzenesulphonic acid) by reacting p-toluidine at 10.degree.-55.degree. C. with oleum in sulphuric acid. The molar ratio of SO.sub.3 to p-toluidine in this reaction is 1-3.0:1. The reaction mixture is worked up by pouring into water and filtering off the precipitated p-toluidine-2-sulphonic acid.

    摘要翻译: 以非常纯的形式获得对甲苯胺-2-磺酸(5-氨基-2-甲基苯磺酸),实际上不含对甲苯胺-3-磺酸(2-氨基-5-甲基苯磺酸) 甲苯胺在10 -55℃下与发烟硫酸在硫酸中反应。 该反应中SO 3与对甲苯胺的摩尔比为1-3.0:1。 将反应混合物倒入水中并滤出沉淀的对甲苯胺-2-磺酸。

    Process for the preparation of 1-amino-8-naphthol-4,6-disulphonic acid
(k-acid)
    39.
    发明授权
    Process for the preparation of 1-amino-8-naphthol-4,6-disulphonic acid (k-acid) 失效
    制备1-氨基-8-萘酚-4,6-二磺酸(k-酸)的方法

    公开(公告)号:US4609503A

    公开(公告)日:1986-09-02

    申请号:US195024

    申请日:1980-10-08

    CPC分类号: C07C303/22

    摘要: The invention relates to a process for the preparation of 1-amino-8-naphthol-4,6-disulphonic acid (K-acid) as the mono-alkali metal salt by reacting a mixture of naphthylaminetrisulphonic acids and/or salts thereof with an alkali metal salt solution and separating the K-acid as the mono-alkali metal salt, by acidification and crystallization. The product is a known valuable dyestuff intermediate.

    摘要翻译: 本发明涉及通过使萘基氨基三硫酸和/或其盐与一种碱金属盐的混合物与一种碱金属盐的混合物制备1-氨基-8-萘酚-4,6-二磺酸(K-酸) 碱金属盐溶液,并通过酸化和结晶分离K-酸作为单碱金属盐。 该产品是已知的有价值的染料中间体。

    Preparation of novel 5-acyloxy-4-(5H)-oxazolonium salts suited for use
as intermediates for triazinone herbicides
    40.
    发明授权
    Preparation of novel 5-acyloxy-4-(5H)-oxazolonium salts suited for use as intermediates for triazinone herbicides 失效
    制备适合用作三嗪酮除草剂的中间体的新型5-酰氧基-4-(5H) - 恶唑鎓盐

    公开(公告)号:US4594427A

    公开(公告)日:1986-06-10

    申请号:US360495

    申请日:1982-03-22

    CPC分类号: C07D253/075 C07D263/44

    摘要: Novel 5-acyloxy-4(5H)-oxazolonium salts of the formula ##STR1## in which R.sup.1 represents an optionally substituted aliphatic group with up to 12 carbon atoms, an optionally substituted cycloalkyl group with 3 to 10 carbon atoms, an optionally substituted phenyl or naphthyl group or an optionally substituted heterocyclic group andR.sup.2 and R.sup.3 are identical or different and represent a hydrogen atom or an optionally substituted aliphatic group with up to 8 carbon atoms or an optionally substituted phenyl group andX.sup..crclbar. represents the anion of an inorganic or organic acid having a pK.sub.a value of less than 2,are obtained in solution when an acyl cyanide of the general formulaR.sup.1 --CO--CN (II)is reacted with a carboxylic acid anhydride of the general formulaR.sup.2 --CO--O--CO--R.sup.3 (III)whereinR.sup.1, R.sup.2 and R.sup.3 each have the abovementioned meaning,in the presence of one or more inorganic or organic acids having a pK.sub.a value of less than 2, and if appropriate in the presence of a solvent, and if appropriate at a temperature between 0.degree. and 120.degree. C.The novel oxazolonium salts (I) can be used as intermediate products for the preparation of known, herbicidally active 3,4,6-trisubstituted 1,2,4-triazin-5(4H)-ones.

    摘要翻译: 式(Ⅰ)的新的5-酰氧基-4(5H) - 恶唑盐,其中R 1表示任选取代的具有至多12个碳原子的脂族基团,任选取代的具有3至10个碳原子的环烷基, 任选取代的苯基或萘基或任选取代的杂环基,R2和R3相同或不同,表示氢原子或任选取代的具有至多8个碳原子的脂族基团或任选取代的苯基,X( - )表示 当通式R 1 -CO-CN(II)的酰基氰与通式为R 2 -CO的羧酸酐反应时,溶液中得到pKa值小于2的无机或有机酸的阴离子 在一种或多种pKa值小于2的无机或有机酸的存在下,并且如果在溶剂存在下适当,其中R 1,R 2和R 3各自具有上述含义的-O-CO-R 3(III) ,如果合适的话 在0至120℃之间的温度下,新的恶唑鎓盐(I)可用作中间产物,用于制备已知的除草活性的3,4,6-三取代的1,2,4-三嗪-5(4H )-那些。