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    • 3. 发明授权
    • Process for preparing cyclopropylacetylene
    • 环丙基乙炔的制备方法
    • US06207864B1
    • 2001-03-27
    • US09380382
    • 1999-09-01
    • Michael HenningsenArmin StammMartin FischerWolfgang Siegel
    • Michael HenningsenArmin StammMartin FischerWolfgang Siegel
    • C07C4530
    • C07F9/535C07C1/30C07C17/00C07C17/18C07C2601/02C07C13/04C07C22/00
    • The invention relates to a process for the halogenation of cyclopropylmethyl ketone with at least one dihalo-triorganophosphorane of the general formula I R3PHal2   (I), in which the radicals R can be the same or different and denote a saturated or unsaturated aliphatic C1-C20 hydrocarbon radical, a phenyl or (C1-C4 alkyl)phenyl radical, which may be optionally substituted by one or two fluorine, chlorine and/or nitro groups, P stands for phosphorus and Hal denotes chlorine, bromine, or iodine, at a temperature of from 800° to 130° C., where the dihalo-triorganophosphane of the general formula (I) is synthesized in situ from triorganophosphane oxide or triorganophosphane sulfide of the general formula II R3PA   (II), in which R is as defined above with respect to formula I and A denotes oxygen or sulfur, using a halogenating agent, wherein the triorganophosphane oxide or triorganophosphane sulfide is used in catalytic amounts, to the halogenation product of cyclopropylmethyl ketone obtained in said process, and to a process for the conversion of said halogenation product to cyclopropylacetytene.
    • 本发明涉及用至少一种通式Iin的二卤代三有机基磷烷卤化环丙基甲基酮的方法,其中基团R可以相同或不同,表示饱和或不饱和的脂族C 1 -C 20烃基,苯基或 (C 1 -C 4烷基)苯基,其可任选被一个或两个氟,氯和/或硝基取代,P代表磷,Hal代表氯,溴或碘,温度为800°至130° ℃,其中通式(I)的二卤代三有机膦原位由通式IIin的三有机膦氧化物或三有机磷烷硫化物原位合成,其中R如对于式I所定义,A表示氧或硫,使用 一种卤化剂,其中三有机膦氧化物或三有机基硫化物以催化量使用于在所述方法中获得的环丙基甲基酮的卤化产物,t o将所述卤化产物转化为环丙基乙烯基的方法。
    • 7. 发明授权
    • Process for the preparation of substituted anthraquinones
    • 制备取代蒽醌的方法
    • US6127580A
    • 2000-10-03
    • US200936
    • 1998-11-30
    • Wolfgang SiegelAndreas Kramer
    • Wolfgang SiegelAndreas Kramer
    • C07C46/02C07C45/00
    • C07C46/02
    • Process for the preparation of anthraquinones of the general formula I ##STR1## in which R.sup.1, R.sup.2, R.sup.3 and R.sup.4, which can be identical or different, are hydrogen, a C.sub.1 -C.sub.8 -alkyl or C.sub.2 -C.sub.8 -alkenyl radical, in which 1,4-naphthoquinone is reacted with a 1,3-diene of the general formula II ##STR2## in a cycloaddition step to give the corresponding tetrahydroanthraquinone and the tetrahydroanthraquinone is oxidized with oxygen in the presence of a basic catalyst to give the anthraquinone, in which both the cycloaddition step and the oxidation step are carried out in the presence of an aqueous diluent.Preferably, the cycloaddition step and oxidation step are carried out at a reaction temperature between 90 and 110.degree. C. and at atmospheric pressure.
    • 用于制备通式I的蒽醌的方法,其中可以相同或不同的R 1,R 2,R 3和R 4是氢,C 1 -C 8 - 烷基或C 2 -C 8 - 烯基,其中1,4 萘醌在环加成步骤中与通式II的1,3-二烯反应,得到相应的四氢蒽醌,四氢蒽醌在碱性催化剂存在下用氧氧化得到蒽醌,其中环加成步骤 并且氧化步骤在水性稀释剂的存在下进行。 优选环加成步骤和氧化步骤在90-110℃的反应温度和大气压下进行。
    • 9. 发明授权
    • Process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas
    • 基本上不含无甲酸的N-烷基-N'-甲基亚烷基脲的方法
    • US06554966B1
    • 2003-04-29
    • US09603195
    • 2000-06-26
    • Andreas KramerJohann-Peter MelderHeinz RütterGünter RieweWolfgang SiegelHans-Jürgen Weyer
    • Andreas KramerJohann-Peter MelderHeinz RütterGünter RieweWolfgang SiegelHans-Jürgen Weyer
    • B01D300
    • C07D239/10
    • The invention relates to a process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas of the formula with R1=H or CH3, R2=CnH2n+1 with n=1-4 and x=0 or 1, from the corresponding alkyleneureas by reaction with monomeric or polymerized formaldehyde in the presence of formic acid. This entails feeding the mixture, obtained in the reaction, of N-alkyl-N′-methylalkyleneurea and formic acid to the upper region of a distillation column, distilling without further additions and removing essentially formic acid-free N-alkyl-N′-methylalkyleneurea in the lower region of the column. The process parameters are set so that the pressure in the upper region of the column is at a higher level than in the lower region of the column, and the difference in pressure between the upper and lower regions of the column is from 10 to 100 mbar, and the temperature in the lower region of the column is higher than in the upper region of the column, with the difference in temperature between the upper and lower regions of the column being from 40° C. to 210° C.
    • 本发明涉及一种制备基本上无甲酸的N-烷基-N'-甲基亚烷基脲的方法,其中R1 = H或CH3,R2 = CnH2n + 1,其中n = 1-4和x = 0或1, 通过在甲酸存在下与单体或聚合的甲醛反应来制备相应的亚烷基脲。 这需要将N-烷基-N'-甲基亚烷基脲和甲酸的反应混合物加入到蒸馏塔的上部区域,无需进一步添加即可蒸馏除去基本上不含甲酸的N-烷基-N'- 甲基亚烷基脲在柱的下部区域。 设定工艺参数使得塔的上部区域中的压力处于比塔的下部区域更高的水平,并且塔的上部和下部区域之间的压力差为10至100mbar ,塔的下部区域的温度高于塔的上部区域,塔的上部和下部区域之间的温度差为40℃〜210℃。