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胺化

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The invention adopts halogen acetylized crosslinked polystyrene resin and hydroxybenzyl alcohol as the raw material, and the solid phase synthesis carrier with hydroxymethyl as the active group is synthesized through the joint catalysis of N, N-dimethyl formamide used as the reaction solvent, inorganic base and phase-transfer catalyst.

本发明采用卤乙酰化交联聚苯乙烯树脂和对羟基苯甲醇为原料,在以N,N-二甲基甲酰胺为反应溶剂、无机碱及相转移催化剂的共同催化下合成了一种以羟甲基为活性基团的固相合成载体。

In the third step, when the ratio of racemic ester to benzenesulfonyl chloride to triethylamine to catalyst 4-DMAP is 1:1:1:0.1 in 10℃, the yield is 82.9% and high purity is obtained by crystallisation.

在第三步磺酰化反应中,得到合成消旋2-苯磺酸基-2(2-氯苯基)乙酸甲酯的较佳反应条件为邻氯扁桃酸甲酯:苯磺酰氯:三乙胺=1:1:1,催化剂4-DMAP用量为摩尔反应物的10%,反应温度为10℃,收率为82.9%,同时用结晶方法获得高纯度的产物。

Onset decomposition temperature of the polyimide was at 508 ℃ under nitrogen atmosphere, and its glass-transition temperature was at 288 ℃. The polyimide film had strengths at break at 91 MPa, elongations to break of 10%~15%, and initial moduli at 1.7 GPa.

此外该聚醚酰亚胺还表现出良好的热性能和机械性能:玻璃化转变温度在288 ℃,氮气中起始分解温度在508 ℃;该聚合物薄膜的拉伸强度为91 MPa,断裂伸长率在10%~15%,起始模量为1.7 GPa。

Optimum conditions are as follows: DMF is used as solvent, compound quaternary ammonium salt as catalyst, n(p-nitrochloro benzene):n=1: 1.2, m:m(p-nitrochloro benzene)=4%, m:m(p-nitrochloro benzene)1:1, and reacted under 155~160℃ for 18 h; reduction reaction is carried out in methanol with Raney nickel, which is used as catalyst; the raw product is added an antioxidant, and distilled simply under reduced pressure to obtain 4-fluoroaniline with excellence quality, purity is over 99.5%, total yield is 89.3%.

实验结果表明,氟化反应的最佳条件为:二甲基甲酰胺为溶剂、复合季铵盐为催化剂,n:n=1:1.2,m(催化剂:m=4%,m:m=1:1,于155~160℃下反应18h;还原反应在甲醇中进行,以阮内镍为催化剂;粗产品加入抗氧剂,减压条件下简单蒸馏得高品位的对氟苯胺。

Objective To investigate the effects of subthalamic nucleus -deep brain stimulation on expression of dopamine and adenosine 3'5'-monophosphate-regulated phosphor-protein (DARPP-32) and its phosphorylated proteins in corpus striatum of rat models with levodopa-induced dyskinesia.

目的 探讨丘脑底核高频电刺激对帕金森病异动症大鼠纹状体区多巴胺和cAMP调节的磷蛋白(DARPP-32)及其磷酸化蛋白表达的影响。

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