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    • 1. 发明申请
    • α,ω-ALLYL TERMINATED LINEAR POLY(METHACRYLIC ACID) MACROMONOMERS FOR END-LINKED HYDROGELS AND METHOD OF PREPARATION
    • 用于末端连接氢键的α,ω-ALLYL终止线性聚(甲基丙烯酸)大分子和制备方法
    • WO2003101934A1
    • 2003-12-11
    • PCT/US2002/017636
    • 2002-06-03
    • THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORKKOBERSTEIN, Jeffrey, T.VOJTOVA, LucyTURRO, Nicholas, J.
    • KOBERSTEIN, Jeffrey, T.VOJTOVA, LucyTURRO, Nicholas, J.
    • C07C229/06
    • C08F299/00C08F8/12C08F20/12C08F220/14C08F2220/1825C08F2438/01C08F2810/20C08F120/18
    • Disclosed is a method for making α,ω-allyl terminated macromonomers comprising a plurality of units of an α,β-unsaturated carboxylic acid. The method comprises forming a first mixture containing an ester of an α,β-unsaturated carboxylic acid, a radical initiator comprising an allyl group and a halogen, and a catalyst comprising a transition metal complex. The ester of the α,β-unsaturated carboxylic acid is an ester capable of reacting with a mixture comprising trifluoroacetic acid (TFA) to form the α,β-unsaturated carboxylic acid. The mixture is stirred to form a second mixture containing an α-allyl,ω-halogen-terminated macromonomer comprising a plurality of units of the ester of the α,β-unsaturated carboxylic acid. A third mixture comprising a compound containing at least one transferable allyl group is then added to the second mixture to form a fourth mixture containing a first α,ω-allyl terminated macromonomer comprising a plurality of units of the ester of the α,β-unsaturated carboxylic acid. The first α,ω-allyl terminated macromonomer is separated from the fourth mixture and is mixed with a mixture containing TFA to form a fifth mixture containing the α,ω-allyl terminated macromonomer comprising a plurality of units of the α,β-unsaturated carboxylic acid. The α,ω-allyl terminated macromonomer comprising a plurality of units of the α,β-unsaturated carboxylic acid is then separated from the fifth mixture. Also enclosed is a related method for making end-linked hydrogels comprising a plurality of units of an α,β-unsaturated carboxylic acid. The method comprises forming a first mixture containing an α,ω-allyl terminated macromonomer comprising a plurality of units of the α,β-unsaturated carboxylic acid and a radical initiator. The first mixture is treated with UV-radiation, visible light, or heat to form a second mixture comprising an end-linked hydrogel comprising a plurality of units of the α,β-unsaturated carboxylic acid.
    • 公开了一种制备包含多个α,β-不饱和羧酸单元的α,ω-烯丙基封端的大分子单体的方法。 该方法包括形成含有α,β-不饱和羧酸的酯,包含烯丙基和卤素的自由基引发剂和包含过渡金属络合物的催化剂的第一混合物。 α,β-不饱和羧酸的酯是能够与包含三氟乙酸(TFA)的混合物反应以形成α,β-不饱和羧酸的酯。 将混合物搅拌以形成包含α-烯丙基,ω-卤素封端的大分子单体的第二混合物,其包含多个α,β-不饱和羧酸的酯单元。 然后将包含至少一个可转移的烯丙基的化合物的第三混合物加入到第二混合物中以形成包含第一个α,ω-烯丙基封端的大分子单体的第四混合物,其包含多个单位的α,β-不饱和的 羧酸。 将第一个α,ω-烯丙基封端的大分子单体与第四混合物分离,并与含有TFA的混合物混合以形成包含α,ω-烯丙基封端的大分子单体的第五混合物,其包含多个单位的α,β-不饱和羧酸 酸。 然后将包含多个α,β-不饱和羧酸单元的α,ω-烯丙基封端的大分子单体与第五混合物分离。 还包括用于制备包含多个α,β-不饱和羧酸单元的端联水凝胶的相关方法。 该方法包括形成包含α,ω-烯丙基封端的大分子单体的第一混合物,其包含多个α,β-不饱和羧酸单元和自由基引发剂。 用UV辐射,可见光或加热处理第一混合物以形成第二混合物,其包含包含多个α,β-不饱和羧酸单元的端基水凝胶。