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    • 3. 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℃。
    • 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。