Process for the preparation of pivaloylacetic acid esters
    31.
    发明授权
    Process for the preparation of pivaloylacetic acid esters 失效
    新戊酰乙酸酯的制备方法

    公开(公告)号:US4661621A

    公开(公告)日:1987-04-28

    申请号:US686188

    申请日:1984-12-26

    CPC分类号: C07C69/716

    摘要: An improved process for the preparation of pivaloylacetic acid esters by decarbonylation of pivaloylpyruvic acid esters at elevated temperatures is described. The process is carried out in the presence of 0.01 to 5 percent by weight of a metal of sub-groups one to eight of the periodic system, which metal is in metallic and/or oxidic form. Initially, 30 percent of the pivaloylpyruvic acid ester to be converted is heated in the presence of the metal, and after conversion of the same there is added additional pivaloylpyruvic acid ester according to the rate at which the pivaloylpyruvic acid ester is converted.

    摘要翻译: 描述了通过在升高的温度下对新戊酰丙酮酸酯进行脱羰来制备新戊酰乙酸酯的改进方法。 该方法在0.01至5重量%的周期性系统中一至八个亚组的金属的存在下进行,该金属为金属和/或氧化形式。 最初,在金属存在下,将30%的待转化的新戊酰丙酮酸酯加热,转化后,加入新戊酰丙酮酸酯,根据转化新戊酰丙酮酸酯的速度加入新戊酰丙酮酸酯。

    Process for isolating H acid and K acid
    34.
    发明授权
    Process for isolating H acid and K acid 失效
    H酸和K酸分离方法

    公开(公告)号:US4426334A

    公开(公告)日:1984-01-17

    申请号:US368194

    申请日:1982-04-14

    CPC分类号: C07C303/44

    摘要: The invention relates to a process for isolating H acid and K acid in the form of their monoalkali metal salts from acid aqueous solutions which contain these two acids and alkali metal ions and may contain other aminonaphtholdisulphonic acids, in which process H acid monoalkali metal salts are precipitated at elevated temperatures from solutions which contain not only sodium ions but also potassium ions and then precipitating K acid monoalkali metal salts by cooling down the filtrate obtained after separating off the H acid monoalkali metal salts.

    摘要翻译: 本发明涉及一种从含有这两种酸和碱金属离子的酸性水溶液中分离其单碱金属盐形式的H酸和K酸的方法,并且可以含有其它氨基十氢四氢呋喃磺酸,其中H酸单碱金属盐为 在不仅含钠离子和钾离子的溶液中在高温下沉淀,然后通过冷却分离H酸单碱金属盐后得到的滤液而沉淀K酸单碱金属盐。

    Preparation of
4-amino-6-tert.-butyl-3-alkylthio-1,2,4-triazin-5-(4H)-ones
    35.
    发明授权
    Preparation of 4-amino-6-tert.-butyl-3-alkylthio-1,2,4-triazin-5-(4H)-ones 失效
    制备4-氨基-6-叔丁基-3-烷硫基-1,2,4-三嗪-5-(4H) - 酮

    公开(公告)号:US4328340A

    公开(公告)日:1982-05-04

    申请号:US235496

    申请日:1981-02-19

    IPC分类号: C07D253/06 C07D253/075

    CPC分类号: C07D253/075

    摘要: In the preparation of 4-amino-6-tert.-butyl-3-methylthio-1,2,4-triazin-5-(4H)-one of the formula ##STR1## wherein pivaloyl cyanide of the formula(CH.sub.3).sub.3 C--CO--CNis reacted to form an intermediate, the intermediate is condensed with thiocarbohydrazide of the formulaNH.sub.2 --NH--CS--NH--NH.sub.2to form 4-amino-6-tert.-butyl-3-mercapto-1,2,4-triazin-5-(4H)-one of the formula ##STR2## and the 4-amino-6-tert.-butyl-3-mercapto-1,2,4-triazin-5-(4H)-one is alkylated to replace the H atom on the sulphur by --C.sub.1-4 --alkyl, the improvement which comprises reacting the pivaloyl cyanide with a carboxylic acid anhydride of the formulaR--CO--O--CO--Rin which R is an optionally substituted aliphatic radical with up to 8 carbon atoms or an optionally substituted phenyl radical, in the presence of a strong acid at a temperature between about -50.degree. and +150.degree. C., and then directly reacting the reaction mixture thus obtained with the thiocarbahydrazide. Advantageously R is CH.sub.3, the strong acid is concentrated sulphuric acid, the pivaloyl cyanide is effected at a temperature between about 0.degree. and 100.degree. C., the condensation with thiocarbohydrazide is effected, in the presence of a mineral acid, in an aqueous or aqueous-alcoholic medium, and the alkylation is effected using methyl iodide or methyl bromide in the presence of sodium hydroxide at about 0.degree. to 50.degree. C.

    摘要翻译: 在制备式(CH 3)3 C的新戊酰基氰的4-氨基-6-叔丁基-3-甲硫基-1,2,4-三嗪-5-(4H) - 酮中, -CO-CN反应形成中间体,中间体与式NH 2 -NH-CS-NH-NH 2的硫代碳酰肼缩合形成4-氨基-6-叔丁基-3-巯基-1,2, (4H) - 酮和4-氨基-6-叔丁基-3-巯基-1,2,4-三嗪-5-(4H) - 酮是 烷基化以用-C 1-4烷基取代硫上的H原子,其改进包括使新戊酰氰与式R-CO-O-CO-R的羧酸酐反应,其中R是任选取代的脂族 具有多达8个碳原子的基团或任选取代的苯基,在强酸存在下,在约-50至+ 150℃之间的温度下,然后将由此获得的反应混合物与硫代碳酰肼直接反应。 有利地,R是CH 3,强酸是浓硫酸,新戊酰氰在约0℃至100℃的温度下进行,与硫代碳酰肼的缩合在无机酸的存在下,在水或 水性醇介质,在氢氧化钠存在下,在约0〜50℃下,使用甲基碘或甲基溴进行烷基化。

    Process for the preparation of sulfonic acid chlorides
    37.
    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
    38.
    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 1,5-dihydroxynaphthalene and
1,5-diaminonaphthalene
    39.
    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。