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    • 4. 发明申请
    • PROCESS FOR THE CONTINUOUS PRODUCTION OF 3,3'-DICHLORO-BENZIDINE DIHYDROCHLORIDE
    • 连续生产3,3'-二氯 - 二苯并二氢氯化物的方法
    • WO1991007377A1
    • 1991-05-30
    • PCT/EP1990001844
    • 1990-11-03
    • HOECHST AKTIENGESELLSCHAFTHABIG, KurtBAESSLER, KonradWARNING, Klaus
    • HOECHST AKTIENGESELLSCHAFT
    • C07C209/54
    • C07C209/54
    • Process for the continuous production of 3,3'-dichloro-benzidine dihydrochloride from 2-2'-dichloro-hydrazobenzole by treatment with aqueous sulphuric acid by continuously adding to the 2-2'-dichlorohydrazobenzole dissolved in an aromatic solvent which is not miscible with water, at about 20 to 50 DEG C in the presence of an alkaline metal salt of an alkyl(C8-C23) polyglycol ether sulphate, such a quantity of 50 to 80 % aqueous sulphuric acid that the suspension formed remains transportable and then also continuously diluting the suspension emerging from the reaction region with water and heating it to about 90 to 95 DEG C until a solution is obtained, separating the aromatic solvent from the hot sulphuric acid aqueous phase, causing the 3-3'-dichloro-benzidine dihydrochloride to precipitate by the addition of hydrochloric acid to the remaining sulphuric acid solution and filtering it.
    • 通过连续加入溶解在不溶混的芳族溶剂中的2-2'-二氯联苯甲醇,通过用硫酸水溶液连续生产3,3'-二氯 - 联苯胺二盐酸盐的方法 在约20至50℃下,在烷基(C 8 -C 23)聚乙二醇醚硫酸盐的碱金属盐存在下,使得所形成的悬浮液的50-80%硫酸水溶液仍然可运输,然后也 用水连续稀释反应区域的悬浮液,加热至约90〜95℃,直至得到溶液,将芳族溶剂与热硫酸水相分离,得到3-3'-二氯联苯胺二盐酸盐 通过向剩余的硫酸溶液中加入盐酸进行沉淀并过滤。
    • 8. 发明申请
    • A PROCESS FOR SEPARATING O- AND P-SUBSTITUTED BENZENE COMPOUNDS
    • 用于分离O-和P-取代的苯甲醛化合物的方法
    • WO02010097A1
    • 2002-02-07
    • PCT/IN2000/000072
    • 2000-07-27
    • C07B61/00C07B63/00C07C45/79C07C45/80C07C51/42C07C51/47C07C209/54C07C211/51C07C37/68C07C45/78C07C201/16C07C209/82C07C221/00C07C227/38
    • C07C209/54C07B63/00C07C45/79C07C45/80C07C51/42C07C51/47C40B40/00C07C49/825C07C47/565C07C63/10C07C65/30C07C211/51
    • A process for producing o- and p- substituted benzene compounds separately from a binary mixture in any proportions of said compounds. The said o- and p- substituted benzene compounds comprise isomeric 1,2 substituted benzene compound of Formula (1) and 1,4 substituted benzene compound of Formula (2) respectively, wherein R1 is selected from the group of -OH, -COOH, -NH2, N(R3)(R4) where R3 and R4 are from the group -H, (CH2)nCH3; n=0-4; and R2 is selected from the group consisting of -(CO-CH3), -(NH2), -(OH), -(NO2), -(X), -(OCH3), -COOH, -CHO, -(OCH2CH3) and X is halogen selected from F, CL, Br and I. The process basically involves (i) treating the said binary mix first with an organic solvent to phase separate by preferential solubilisation one of the said two compounds, (ii) contacting the solution phase with an ion exchange resin for preferentially adsorbing and recovering further any of said undissolved compound present to thereby further phase separate from the said compound in said solution phase the other compound as substantially pure undissolved compound, and (iii) recovering from the said solution phase of step (ii) above the said soluble compound in substantially pure form by desolventising the solution phase in conventional manner. The process provides for simple and cost effective method of producing pure compounds of Formula (1) and Formula (2) separately in high yield.
    • 与所述化合物的任何比例的二元混合物分开生产邻位和对位取代的苯化合物的方法。 所述邻取代和取代的苯化合物分别包含式(1)的异构1,2-取代的苯化合物和式(2)的1,4取代的苯化合物,其中R 1选自-OH,-COOH ,-NH 2,N(R 3)(R 4)其中R 3和R 4来自基团-H,(CH 2)n CH 3; N = 0-4; 并且R2选自 - (CO-CH3), - (NH2), - (OH), - (NO2), - (X), - (OCH3),-COOH,-CHO, - (OCH2CH3 ),X是选自F,CL,Br和I的卤素。该方法基本上包括(i)首先用有机溶剂处理所述二元混合物,以通过优先溶解所述两种化合物之一相分离,(ii) 溶液相与离子交换树脂进一步优先吸附和回收存在的所述未溶解化合物,从而进一步与所述溶液相中的所述化合物相分离,将另一种化合物作为基本上纯的未溶解化合物,和(iii)从所述溶液中回收 通过以常规方式去溶解溶液相,基本上纯的形式在所述可溶性化合物上方的步骤(ii)的相。 该方法提供了以高产率分别生产式(1)和式(2)的纯化合物的简单且成本有效的方法。