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    • 6. 发明申请
    • BATCH PROCESS FOR THE PREPARATION OF CIS-2,2,4,4-TETRAMETHYLCYCLOBUTANE-1,3-DIOL
    • 制备CIS-2,2,4,4-四甲基胆甾烷-1,3-二醇的批处理方法
    • WO2016094479A1
    • 2016-06-16
    • PCT/US2015/064624
    • 2015-12-09
    • EASTMAN CHEMICAL COMPANY
    • STAVINOHA, Jerome, Leonard, Jr.ASHCROFT, Carey, DanHOYME, Craig, AlanKELLY, Kelmara, Khadene
    • C07C29/56C07C29/145C07C35/04
    • C07C29/145C07B2200/09C07C29/56C07C2601/04C07C35/045
    • This invention is generally directed to a batch process for the preparation of cis-2,2,4,4-tetramethylcyclobutane-1,3-diol comprising: (A) treatment of at least one monomer selected from 2,2,4,4- tetramethylcyclobutane-1,3-dione, 3-hydroxy-2, 2,4,4- tetramethylcyclobutanone, and 2,2,4,4-tetramethylcyclobutane-1,3-diol said diol having a starting cis:trans molar ratio of 0:1 to about 2:1, or mixtures thereof by contacting said monomer(s) with hydrogen in the presence of a reaction solvent in which the resulting cis-2, 2,4,4- tetramethylcyclobutane-1,3-diol is partially soluble and further in the presence of a catalyst comprising about 0.1 to about 10 weight percent ruthenium, based on the total weight of the catalyst, deposited on a support material, under reaction conditions sufficient to produce a cis- 2,2,4,4-tetramethylcyclobutane-1,3-diol having a final cis:trans molar ratio of from 2:1 to about 25:1; (B) removal of the reaction solvent, whether by filtration, centrifugation, or other methods known to one of ordinary skill in the art; (C) dissolution of the 2,2,4,4-tetramethylcyclobutane-1,3-diol with at least one solvent; and, optionally, (D) washing the catalyst at least once, and optionally, (E) reuse of the catalyst.
    • 本发明一般涉及制备顺式-2,2,4,4-四甲基环丁烷-1,3-二醇的分批方法,其包括:(A)处理至少一种选自2,2,4,4 - 四甲基环丁烷-1,3-二酮,3-羟基-2,2,4,4-四甲基环丁酮和2,2,4,4-四甲基环丁烷-1,3-二醇,所述二醇具有起始顺式:反式摩尔比 0:1至约2:1,或其混合物通过在反应溶剂存在下使所述单体与氢接触,其中所得顺式-2,4,4-四甲基环丁烷-1,3-二醇为 在足以产生顺式-2,2,4或4的反应条件下,在包含约0.1至约10重量%的催化剂的催化剂存在下,基于沉积在载体材料上的催化剂的总重量, 具有最终顺式:反式摩尔比为2:1至约25:1的4-四甲基环丁烷-1,3-二醇; (B)通过过滤,离心或本领域普通技术人员已知的其它方法除去反应溶剂; (C)使用至少一种溶剂使2,2,4,4-四甲基环丁烷-1,3-二醇溶解; 和(D)将催化剂洗涤至少一次,任选地(E)催化剂的再利用。