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    • 7. 发明授权
    • Process for preparing alkyl- and arylmalonic acids
    • 制备烷基和芳基丙二酸的方法
    • US5849949A
    • 1998-12-15
    • US64005
    • 1998-04-21
    • Klaus-Dieter Steffen
    • Klaus-Dieter Steffen
    • C07C27/02C07C51/09C07C51/48C07C55/02C07C57/36C07C61/04C07C61/09C07C51/00
    • C07C51/09
    • Alkyl- and arylmalonic acids of the formula I ##STR1## where R.sup.1 =H, C.sub.1 -C.sub.12 -alkyl, phenyl, C.sub.1 -C.sub.4 -alkylphenyl, C.sub.2 -C.sub.4 -dialkylphenyl, R.sup.2 =C.sub.1 -C.sub.12 -alkyl, phenyl, C.sub.1 -C.sub.4 -alkylphenyl, C.sub.2 -C.sub.4 -dialkylphenyl or R.sup.1 +R.sup.2 =--CH.sub.2 --CH.sub.2 --, are prepared by alkaline saponification by hydrolyzing the corresponding C.sub.1 -C.sub.4 -alkyl esters of the malonic acid of formula I, with alkali metal hydroxide dissolved in an aqueous alkali metal salt solution containing salt at 90-100% of saturation, acidifying the hydrolysis product with a mineral acid, removing the precipitated alkali metal salt which forms upon acidification, and extracting the alkyl- and arylmalonic acid formed from the aqueous solution with the aid of an organic solvent.
    • 式I的烷基和芳基丙二酸(I)其中R1 = H,C1-C12-烷基,苯基,C1-C4-烷基苯基,C2-C4-二烷基苯基,R2 = C1-C12-烷基,苯基, C 1 -C 4 - 烷基苯基,C 2 -C 4 - 二烷基苯基或R 1 + R 2 = -CH 2 -CH 2 - ,是通过碱溶解通过水解相应的式I的丙二酸的C 1 -C 4烷基酯与碱金属氢氧化物 在含有90-100%饱和盐的碱金属盐水溶液中,用无机酸酸化水解产物,除去在酸化时形成的沉淀的碱金属盐,并提取由水溶液形成的烷基和芳基丙二酸 借助有机溶剂。
    • 8. 发明授权
    • Process for preparing n-alkyllactams
    • 制备正烷基内酰胺的方法
    • US5508396A
    • 1996-04-16
    • US421237
    • 1995-04-13
    • Klaus-Dieter Steffen
    • Klaus-Dieter Steffen
    • C07D207/26C07D207/267C07D227/08C07D223/06
    • C07D207/267C07D227/08Y02P20/582
    • A process for preparing an N-alkyllactam, comprising the steps of:(a) reacting a lactam with an alkali metal alkoxide at 130.degree.-170.degree. C. and removing the alcohol formed by distillation;(b) reacting the product from step (a), if desired in a mixture with the product from step (e), with an alkyl halide in a solvent which is(i) an ethylene glycol dialkyl ether of the formula R--O--(CH.sub.2 --CH.sub.2 --O).sub.m R, where R in C.sub.1 -C.sub.4 -alkyl and m is 1-8,(ii) the N-alkyllactam to be prepared or(iii) a mixture of (i) and (ii), to obtain crude N-alkylactam or an alkali metal salt;(c) separating the alkali metal salt from the crude N-alkylactam;(d) subjecting the N-alkyllactam crude product to high-purity distillation after addition of a sufficient amount of alkali metal alkoxide to convert any unreacted lactam to a salt; and(e) recycling the bottom product of the distillation in step (d) in step (e) into step (b), is environmentally friendly and affords the desired N-alkyllactam in high yield and high purity.
    • 一种制备N-烷基内酰胺的方法,包括以下步骤:(a)使内酰胺与碱金属醇盐在130-170℃反应并除去通过蒸馏形成的醇; (b)如果需要,与步骤(e)的产物的混合物中的步骤(a)的产物与烷基卤化物在溶剂中反应,所述溶剂是(ⅰ)式RO-(CH 2 -CH 2 -O)m R,其中C 1 -C 4烷基中的R和m为1-8,(ii)待制备的N-烷基内酰胺或(iii)(i)和(ii)的混合物,得到粗品 N-烷基内酰胺或碱金属盐; (c)从粗N-烷基内酰胺中分离碱金属盐; (d)在加入足够量的碱金属醇盐之后使N-烷基内酰胺粗产物进行高纯度蒸馏以将任何未反应的内酰胺转化为盐; 和(e)将步骤(d)中的步骤(d)中的蒸馏的底部产物再循环到步骤(b)中是环境友好的,并以高产率和高纯度提供所需的N-烷基内酰胺。