Preparation of novel 5-acyloxy-4 (5H)-oxazolonium salts suited for use
as intermediates for triazinone herbicides
    23.
    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:US4980479A

    公开(公告)日:1990-12-25

    申请号:US427162

    申请日:1989-10-25

    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--N (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.

    5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one
    24.
    发明授权
    5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one 失效
    5,5-二氯-4,5-二氢-6-羟基-2-三氯甲基嘧啶-4-酮

    公开(公告)号:US4668788A

    公开(公告)日:1987-05-26

    申请号:US766586

    申请日:1985-08-19

    CPC分类号: C07D239/30 C07D239/553

    摘要: The new compound 5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one can be prepared by reacting 4,6-dihydroxy-2-methylpyrimidine or chlorinated subsequent stages with a chlorinating agent. 5,5-dichloro-4,5-dihydro-6-hydroxy-2-trichloromethylpyrimidin-4-one can be used as an intermediate for the preparation of 2-trichloromethyl-4,5,6-trichloropyrimidine.

    摘要翻译: 新化合物5,5-二氯-4,5-二氢-6-羟基-2-三氯甲基嘧啶-4-酮可以通过使4,6-二羟基-2-甲基嘧啶或氯化后续阶段与氯化剂反应来制备。 5,5-二氯-4,5-二氢-6-羟基-2-三氯甲基嘧啶-4-酮可以用作制备2-三氯甲基-4,5,6-三氯嘧啶的中间体。

    Process for the preparation of pivaloylacetic acid esters
    25.
    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
    28.
    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
    29.
    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。