申请人:PolyMASC Pharmaceuticals plc
公开号:EP1026171A1
公开(公告)日:2000-08-09
A process for producing an adduct of a polymer and a target material which process comprises the steps of
(a) reacting tresyl chloride with a polymer of formula (II)
(C)c POL - Gg (II)
wherein
POL is a polymer moiety of valency c+g,
C is a capping group and c is zero or a positive number and
G is a terminal hydroxyl group reactive with the compound of formula (I) and g is a positive number
so as to form
a sulphonate ester-activated polymer of formula (III)
(C)c POL - (tresyl)g (III)
wherein
C, POL, -AM, c and g are as defined above
(b) reacting the activated polymer of formula (III) with the target material and
(c) recovering the adduct of the polymer and the target material,
in which process:
(i) the polymer of formula (II) is dry as determined by benzene distillation, and
(ii) the reaction of the tresyl chloride with the polymer of formula (II) is conducted in an organic solvent which is inert to the reagents and to the product of formula (III) and is anhydrous as obtainable using molecular sieves of 0.3nm;
(iii) the reaction of the tresyl chloride with the polymer of formula (II) is conducted in a reaction vessel from which water is excluded;
(iv) the activated polymer of formula (III) so produced is recovered and either used directly in step (b) or stored, prior to use in step (b), in the presence of a desiccating agent more hygroscopic than the product of formula (III); and
v) the reaction of the activated polymer with the target material is conducted in a non-denaturing medium and non-denaturing temperature with respect to the target material.
一种生产聚合物和目标材料加合物的工艺,该工艺包括以下步骤
(a) 使甲酰氯与式 (II) 的聚合物反应
(C)c POL - Gg (II)
其中
POL 是化合价为 c+g 的聚合物分子、
C 是封端基团,c 为零或正数,以及
G 是与式 (I) 化合物反应的末端羟基,g 为正数
从而形成
式(III)的磺酸酯活性聚合物
(C)c POL - (甲苯基)g (III)
其中
C、POL、-AM、c 和 g 如上定义
(b) 使式(III)的活化聚合物与目标材料反应,并
(c) 回收聚合物与目标材料的加合物、
在该过程中
(i) 根据苯蒸馏法测定,式(II)聚合物是干的,以及
(ii) 甲酰氯与式(II)聚合物的反应在对试剂和式(III)产物惰性且无水的有机溶剂中进行,该有机溶剂可使用 0.3nm 的分子筛获得;
(iii) 三氯甲烷与式(II)聚合物的反应是在不含水的反应容器中进行的;
(iv) 如此制得的式(III)活化聚合物被回收并直接用于步骤(b),或在用于步骤(b)之前, 在比式(III)产物吸湿性更强的干燥剂存在下储存;以及
v) 活性聚合物与目标材料的反应是在非变性介质和相对于目标材料的非变性温度下进行的。