Process for manufacturing substituted 3-pyridylmethyl ammonium bromides
    111.
    发明授权
    Process for manufacturing substituted 3-pyridylmethyl ammonium bromides 有权
    制备取代的3-吡啶基甲基溴化铵的方法

    公开(公告)号:US09096570B2

    公开(公告)日:2015-08-04

    申请号:US13128787

    申请日:2009-11-13

    摘要: A process for manufacturing 5,6-disubstituted-3-pyridylmethyl ammonium bromides (I), wherein Q is a tertiary aliphatic or cyclic, saturated, partially unsaturated or aromatic amine; Z is hydrogen or halogen; Z1 is hydrogen, halogen, cyano or nitro; Y and Y1 are each independently OR1, NR1R2, or when taken together YY1 is —O—, —S— or NR3—; R1 and R2 are each independently hydrogen, C1-C4 alkyl optionally substituted with C1-C4 alkoxy or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms, or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms; R3 is hydrogen or C1-C4 alkyl; comprises the steps of (i) reacting a compound of formula (II), wherein the symbols have the meaning given in formula (I), with bromine in the presence of a radical initiator in a solvent mixture comprising an aqueous phase and an organic phase, where the organic phase comprises a solvent selected from 1,2-dichloroethane, chlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene and tetrachloromethane, and where the pH-value of the aqueous phase is from 3 to

    摘要翻译: 制备5,6-二取代-3-吡啶基甲基溴化铵(I)的方法,其中Q是叔脂族或环状饱和的,部分不饱和的或芳族的胺; Z是氢或卤素; Z1是氢,卤素,氰基或硝基; Y和Y1各自独立地为OR 1,NR 1 R 2,或者当Y Y 1为-O - , - S-或NR 3 - 时。 R 1和R 2各自独立地为氢,任选被C 1 -C 4烷氧基取代的C 1 -C 4烷基或任选被一至三个C 1 -C 4烷基,C 1 -C 4烷氧基或卤素原子取代的苯基,或任选被一至三个 C1-C4烷基,C1-C4烷氧基或卤原子; R3是氢或C1-C4烷基; 包括以下步骤:(i)在自由基引发剂存在下,将包含式(I)中给出的符号的式(II)化合物与溴在含水相和有机相的溶剂混合物中反应, 其中有机相包含选自1,2-二氯乙烷,氯苯,1,2-二氯苯,1,3-二氯苯,1,4-二氯苯和四氯甲烷的溶剂,其中水相的pH值来自 3至<8,得到3-溴甲基-5,6-二取代的吡啶化合物(III),其中Y,Y 1,Z和Z 1具有式(I)中给出的含义,和(ⅱ)使溴化合物 式(III)与叔胺碱Q在溶剂中在约0℃至100℃的温度范围内

    Method for producing 3-trifluromethylphenyl-4-cyanobenzyl ketone
    114.
    发明申请
    Method for producing 3-trifluromethylphenyl-4-cyanobenzyl ketone 有权
    3-三氟甲基苯基-4-氰基苄基酮的制备方法

    公开(公告)号:US20050171373A1

    公开(公告)日:2005-08-04

    申请号:US10512487

    申请日:2003-04-25

    CPC分类号: C07C253/30 C07C255/56

    摘要: A process is described for preparing 3-trifluoromethylphenyl 4-cyanobenzyl ketone by reacting a C1-C2-alkyl 3-trifluoromethylbenzoate with 4-tolunitrile in an aprotic polar solvent or an aprotic polar solvent mixture in the presence of at least an equimolar amount of a base which is selected from potassium alkoxides of primary C1-C4-alkanols.

    摘要翻译: 描述了一种制备3-三氟甲基苯基4-氰基苄基酮的方法,该方法是在非质子传递极性溶剂中使C 1 -C 2 - 2-烷基-3-三氟甲基苯甲酸酯与4-甲苯腈反应,或 在至少等摩尔量的碱的存在下,非质子极性溶剂混合物,其选自原代C 1 -C 4 - 烷醇的醇盐。

    Process for Manufacturing 5-Formyl-Pyridine-2,3-Dicarboxylic Acid Esters
    119.
    发明申请
    Process for Manufacturing 5-Formyl-Pyridine-2,3-Dicarboxylic Acid Esters 有权
    5-甲酰基 - 吡啶-2,3-二羧酸酯的制备方法

    公开(公告)号:US20110245505A1

    公开(公告)日:2011-10-06

    申请号:US13133013

    申请日:2009-12-07

    CPC分类号: C07D213/80

    摘要: A process for manufacturing a 5-formyl-pyridine-2,3-dicarboxylic acid ester (I) wherein Z is hydrogen or halogen; Z1 is hydrogen, halogen, cyano or nitro and R1, R2 are independently C1-C10-alkyl, comprising the steps of (i) reacting a compound of formula (II), wherein the symbols are as in formula (I), with a nitrosation agent (III) R3—O—N═O (III) wherein R3 is C1-C8-alkyl, in the presence of an alkali metal or alkaline earth metal alcoholates or carbonates in a polar aprotic solvent at a temperature of from −45 to 40° C., to obtain an oxime compound (IV) where Z, Z1, R1 and R2 are as in formula (I), and (ii) reacting oxime compound (IV) with an aliphatic C1-C10-aldehyde in the presence of a Lewis acid at a temperature in the range of from 0 to 100° C. The compounds of formula (I) are useful intermediates in the synthesis of herbicidal imidazolinones, like imazamox.

    摘要翻译: 制备其中Z为氢或卤素的5-甲酰基 - 吡啶-2,3-二羧酸酯(I)的方法; Z1是氢,卤素,氰基或硝基,R1,R2独立地是C1-C10-烷基,包括以下步骤:(ⅰ)使符号如式(I)所示的式(ⅱ)化合物与式 在碱金属或碱土金属醇化物或碳酸盐存在下,在极性非质子溶剂中,温度为-45℃的亚硝化剂(III)R3-O-N = O(Ⅲ)其中R3为C1-C8-烷基 至40℃,得到其中Z,Z 1,R 1和R 2如式(I)中的肟化合物(Ⅳ),和(ⅱ)使肟化合物(Ⅳ)与脂族C 1 -C 10 - 醛在 在0至100℃的温度范围内存在路易斯酸。式(I)化合物是合成除草咪唑啉酮如咪唑氧化物的有用中间体。

    Process for Manufacturing Substituted 3-pyridylmethyl Ammonium Bromides
    120.
    发明申请
    Process for Manufacturing Substituted 3-pyridylmethyl Ammonium Bromides 有权
    制备取代的3-吡啶基甲基溴化铵的方法

    公开(公告)号:US20110224433A1

    公开(公告)日:2011-09-15

    申请号:US13128787

    申请日:2009-11-13

    摘要: A process for manufacturing 5,6-disubstituted-3-pyridylmethyl ammonium bromides (I), wherein Q is a tertiary aliphatic or cyclic, saturated, partially unsaturated or aromatic amine; Z is hydrogen or halogen; Z1 is hydrogen, halogen, cyano or nitro; Y and Y1 are each independently OR1, NR1R2, or when taken together YY1 is —O—, —S— or NR3—; R1 and R2 are each independently hydrogen, C1-C4 alkyl optionally substituted with C1-C4 alkoxy or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms, or phenyl optionally substituted with one to three C1-C4 alkyl groups, C1-C4 alkoxy groups or halogen atoms; R3 is hydrogen or C1-C4 alkyl; comprises the steps of (i) reacting a compound of formula (II), wherein the symbols have the meaning given in formula (I), with bromine in the presence of a radical initiator in a solvent mixture comprising an aqueous phase and an organic phase, where the organic phase comprises a solvent selected from 1,2-dichloroethane, chlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene and tetrachloromethane, and where the pH-value of the aqueous phase is from 3 to

    摘要翻译: 制备5,6-二取代-3-吡啶基甲基溴化铵(I)的方法,其中Q是叔脂族或环状饱和的,部分不饱和的或芳族的胺; Z是氢或卤素; Z1是氢,卤素,氰基或硝基; Y和Y1各自独立地为OR 1,NR 1 R 2,或者当Y Y 1为-O - , - S-或NR 3 - 时。 R 1和R 2各自独立地为氢,任选被C 1 -C 4烷氧基取代的C 1 -C 4烷基或任选被一至三个C 1 -C 4烷基,C 1 -C 4烷氧基或卤素原子取代的苯基,或任选被一至三个 C1-C4烷基,C1-C4烷氧基或卤原子; R3是氢或C1-C4烷基; 包括以下步骤:(i)在自由基引发剂存在下,将包含式(I)中给出的符号的式(II)化合物与溴在含水相和有机相的溶剂混合物中反应, 其中有机相包含选自1,2-二氯乙烷,氯苯,1,2-二氯苯,1,3-二氯苯,1,4-二氯苯和四氯甲烷的溶剂,其中水相的pH值来自 3至<8,得到3-溴甲基-5,6-二取代的吡啶化合物(III),其中Y,Y 1,Z和Z 1具有式(I)中给出的含义,和(ⅱ)使溴化合物 式(III)与叔胺碱Q在溶剂中在约0℃至100℃的温度范围内