Batch process for the preparation of cis-2,2,4,4-tetramethylcyclobutane-1,3-diol
    4.
    发明授权
    Batch process for the preparation of cis-2,2,4,4-tetramethylcyclobutane-1,3-diol 有权
    用于制备顺式-2,2,4,4-四甲基环丁烷-1,3-二醇的分批方法

    公开(公告)号:US09238603B1

    公开(公告)日:2016-01-19

    申请号:US14566245

    申请日:2014-12-10

    Abstract: 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.

    Abstract translation: 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,所述二醇的起始顺式:反式摩尔比为 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-2,2,4,4-四甲基环丁烷-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%钌的催化剂存在下进一步沉积在载体材料上的催化剂总重量, 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。

    Process for the preparation of cis-2,2,4,4-tetramethylcyclobutane-1,3-diol
    10.
    发明授权
    Process for the preparation of cis-2,2,4,4-tetramethylcyclobutane-1,3-diol 有权
    顺式-2,2,4,4-四甲基环丁烷-1,3-二醇的制备方法

    公开(公告)号:US09238602B1

    公开(公告)日:2016-01-19

    申请号:US14566154

    申请日:2014-12-10

    Abstract: This invention is generally directed to a process for the preparation of cis-2,2,4,4-tetramethylcyclobutane-1,3-diol comprising: 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.

    Abstract translation: 本发明一般涉及一种制备顺式-2,2,4,4-四甲基环丁烷-1,3-二醇的方法,包括:处理至少一种选自2,2,4,4-四甲基环丁烷-1 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,所述二醇的起始顺式:反式摩尔比为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-2,2,4,4-四甲基环丁烷-1,3-二醇是部分可溶的,并且进一步 在催化剂存在下,在足以产生顺式-2,2,4,4-四甲基环丁烷-1-酮的反应条件下,基于沉积在载体材料上的催化剂的总重量计,约0.1至约10重量%的钌, 1,3-二醇的顺式:反式摩尔比为2:1至25:1。

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