Process for the manufacture of
5-dichloroacetyl-3,3,6-trimethyl-9-oxo-1,5-diazabicyclo�4.3.0! nonane
    5.
    发明授权
    Process for the manufacture of 5-dichloroacetyl-3,3,6-trimethyl-9-oxo-1,5-diazabicyclo�4.3.0! nonane 失效
    制备5-二氯乙酰基-3,3,6-三甲基-9-氧代-1,5-二氮杂双环[4.3.0]壬烷的方法

    公开(公告)号:US5677452A

    公开(公告)日:1997-10-14

    申请号:US736438

    申请日:1996-10-24

    CPC分类号: C07D487/04

    摘要: The manufacture of 5-dichloroacetyl-3,3,6-trimethyl-9-oxo-1,5-diazabicyclo�4.3.0!-nonane I by the reaction of 3,3,6-trimethyl-9-oxo-1,5-diaza-bicyclo�4.3.0!nonane II with dichloroacetyl chloride in the presence of a solvent and a base, wherein a) this reaction is carried out in a two-phase system comprising a virtually water-insoluble organic solvent and water, and sodium or potassium hydroxide acting as the base is metered in at a rate corresponding to the rate of consumption of the dichloroacetyl chloride such that the aqueous phase exhibits a pH of from 7 to 9, and b) the resulting product is separated.

    摘要翻译: 通过使3,3,6-三甲基-9-氧代-1,2-二氢异喹啉的反应制备5-二氯乙酰基-3,3,6-三甲基-9-氧代-1,5-二氮杂双环[4.3.0] 5-二氮杂 - 双环[4.3.0]壬烷II与二氯乙酰氯在溶剂和碱存在下反应,其中a)该反应在包含实际上不溶于水的有机溶剂和水的两相体系中进行, 以对应于二氯乙酰氯的消耗速率的速率计量作为碱的氢氧化钠或氢氧化钾,使得水相的pH为7-9,并且b)分离得到的产物。

    Preparation of cyclohexane-dione derivatives
    6.
    发明授权
    Preparation of cyclohexane-dione derivatives 失效
    环己酮衍生物的制备

    公开(公告)号:US5118856A

    公开(公告)日:1992-06-02

    申请号:US562445

    申请日:1990-08-02

    摘要: A process for the preparation of cyclohexanedione derivatives of the general formula I ##STR1## where R.sup.1 is C.sub.2 -C.sub.8 -alkyl, C.sub.2 -C.sub.8 -alkenyl, C.sub.3 -C.sub.12 -cycloalkyl, C.sub.5 -C.sub.12 -cycloalkyl with 0-4 olefinically unsaturated bonds, C.sub.2 -C.sub.8 -alkylthioalkyl, C.sub.6 -C.sub.12 -bicycloalkyl with 0-3 olefinically unsaturated bonds, unsubstituted or substituted aryl or hetaryl, or a heterocyclic radical of 4 to 7 atoms of which not more than 3 may be hetero-atoms chosen from O, S and N, the radical being saturated or olefinically unsaturated, by reacting an .alpha.,.beta.-unsaturated ketone (II) with a dialkyl malonate in the presence of a base to give the alkoxycarbonylcyclohexenolone or its salt (III) ##STR2## and acylation, hydrolysis and decarboxylation of (III), wherein the .alpha.,.beta.-unsaturated ketone (II) is reacted, in the presence of a base, with the dialkyl malonate in a solvent from which the alcohol liberated from the malonate can be distilled off, the alcohol is distilled off, where appropriate as an azeotrope, the salt of the alkoxycarbonylcyclohexenolone is reacted with a carboxylic acid halide and the product, where appropriate after removal of excess acyl halide, is treated with an acylation catalyst, hydrolyzed and decarboxylated.

    摘要翻译: 制备通式I(I)的环己二酮衍生物的方法,其中R 1是C 2 -C 8 - 烷基,C 2 -C 8 - 烯基,C 3 -C 12 - 环烷基,具有0-4烯属的C 5 -C 12 - 环烷基 不饱和键,C 2 -C 8烷硫基烷基,具有0-3烯属不饱和键的C 6 -C 12 - 双环烷基,未取代或取代的芳基或杂芳基,或其中不超过3的4至7个原子的杂环基可以是选择的杂原子 通过在碱存在下使α,β-不饱和酮(II)与丙二酸二烷基酯反应得到烷氧基羰基环己烯醇或其盐,从O,S和N中选择饱和或烯属不饱和基团(III) 和(III)的酰化,水解和脱羧反应,其中α,β-不饱和酮(II)在碱的存在下与丙二酸二烷基酯在可从其中释放出来的丙二酸酯释放的醇的溶剂中反应 关闭,酒精被蒸馏掉,在适当的地方作为azeo 将烷氧基羰基环己烯醇的盐与羧酸卤化物反应,并且在除去过量酰基卤后适当的产物用酰化催化剂处理,水解和脱羧。

    Process for the purification of 7-chloroquinoline-8-carboxylic acids
    7.
    发明授权
    Process for the purification of 7-chloroquinoline-8-carboxylic acids 失效
    纯化7-氯喹啉-8-羧酸的方法

    公开(公告)号:US5310915A

    公开(公告)日:1994-05-10

    申请号:US915992

    申请日:1992-08-03

    CPC分类号: C07D215/48

    摘要: Purification of 7-chloroquinoline-8-carboxylic acids I ##STR1## (X=H, halogen, lower alkyl group) by recrystallization from lower alcohols which are miscible with water, by carrying the recrystallization in the presence of small amounts of a base.The quinolinecarboxylic acids I are valuable crop protection agents.

    摘要翻译: PCT No.PCT / EP91 / 00143 Sec。 371日期:1992年8月3日 102(e)日期1992年8月3日PCT 1991年1月25日PCT PCT。 出版物WO91 / 11436 日期:1991年8月8日。通过在与水混溶的低级醇中重结晶,通过将重结晶进行重结晶,得到7-氯喹啉-8-羧酸I(X = H,卤素,低级烷基) 存在少量的碱。 喹啉羧酸I是有价值的作物保护剂。

    Preparation of heterocyclic-cyclohexanedione derivatives
    8.
    发明授权
    Preparation of heterocyclic-cyclohexanedione derivatives 失效
    杂环 - 环己基衍生物的制备

    公开(公告)号:US5245041A

    公开(公告)日:1993-09-14

    申请号:US809376

    申请日:1991-12-18

    摘要: A process for the preparation of cyclohexanedione derivatives of the general formula I ##STR1## where R.sup.1 is C.sub.2 -C.sub.8 -alkyl, C.sub.2 -C.sub.8 -alkenyl, C.sub.3 -C.sub.12 -cycloalkyl, C.sub.5 -C.sub.12 -cycloalkyl with 0-4 olefinically unsaturated bonds, C.sub.2 -C.sub.8 -alkylthioalkyl, C.sub.6 -C.sub.12 -bicycloalkyl with 0-3 olefinically unsaturated bonds, unsubstituted or substituted aryl or hetaryl, or a heterocyclic radical of 4 to 7 atoms of which not more than 3 may be hetero-atoms chosen from O, S and N, the radical being saturated or olefinically unsaturated, by reacting an .alpha.,.beta.-unsaturated ketone (II) with a dialkyl malonate in the presence of a base to give the alkoxycarbonylcyclohexenolone or its salt (III) ##STR2## and acylation, hydrolysis and decarboxylation of (III), wherein the .alpha.,.beta.-unsaturated ketone (II) is reacted, in the presence of a base, with the dialkyl malonate in a solvent from which the alcohol liberated from the malonate can be distilled off, the alcohol is distilled off, where appropriate as an azeotrope, the salt of the alkoxycarbonylcyclohexenolone is reacted with a carboxylic acid halide and the product, where appropriate after removal of excess acyl halide, is treated with an acylation catalyst, hydrolyzed and decarboxylated.

    摘要翻译: 制备通式I(I)的环己二酮衍生物的方法,其中R 1是C 2 -C 8 - 烷基,C 2 -C 8 - 烯基,C 3 -C 12 - 环烷基,具有0-4烯属的C 5 -C 12 - 环烷基 不饱和键,C 2 -C 8烷硫基烷基,具有0-3烯属不饱和键的C 6 -C 12 - 双环烷基,未取代或取代的芳基或杂芳基,或其中不超过3的4至7个原子的杂环基可以是选择的杂原子 通过在碱存在下使α,β-不饱和酮(II)与丙二酸二烷基酯反应得到烷氧基羰基环己烯醇或其盐,从O,S和N中选择饱和或烯属不饱和基团(III) 和(III)的酰化,水解和脱羧反应,其中α,β-不饱和酮(II)在碱的存在下与丙二酸二烷基酯在可从其中释放出来的丙二酸酯释放的醇的溶剂中反应 关闭,酒精被蒸馏掉,在适当的地方作为azeo 将烷氧基羰基环己烯醇的盐与羧酸卤化物反应,并且在除去过量酰基卤后适当的产物用酰化催化剂处理,水解和脱羧。