文档介绍：郑州大学顾L学位论文
2. 催化剂可以通过简单的过滤、溶剂洗涤进行回收,循环使用五次产率略有下降。
3. 研究了Si02负载环钯化合物催化剂对小同反应底物的偶联反应,得到了较为满
意的结果。并通过熔点、红外光谱和1H NMR测定对产物进行了结构确证。
、表征及其在Heck反应中的催化性能研究
1. 通过硅烷化试剂将Si02表面改性后,与水杨醛作用形成具有配位性能的席夫碱,再与Pd(OAc)2反应得到Si02负载钯配合物催化剂,通过FT-IR、XRD、 TG—DSC以及XPS等手段对配体及催化剂进行了表征。并提出钯配合物的可能结构。
I
一 H毋 3 一 O —一~ O 一占一(CH2)3NH:.Pd(。A。)2si——NH2。Pd(OA。)2
仄/莹+脍i
I甄I
C●、 l
∞^ k\●:
2. 研究了该催化剂对碘代苯与丙烯酸交叉偶联反应的催化性能,考察了不同条件对该反应的影响。得出最适宜反应条件:,碘代苯丙烯酸摩尔比为l:。三乙胺27mmol,,在6mL乙醇溶剂中,83。C下反应 ,%,催化剂循环使用五次之后产率没有明显下降,%。该催化剂对其它反应底物的催化性能也进行了探索。
关键诃:si02负载;环钯化合物;钯配合物;Heck偶联反应;催化剂
郑州大学硕I二学位论文
Abstract
In this paper,we made a detailed review ofrecent development ofHeck reaction and its catalyst,especially palladacycle catalysts and Si02一supported palladium catalyst. There are many Si—OH on the surface of anic silica material,thus,a wide variety of novel hybrid materials with the capability of coordination call be prepared through chemical modification of silica anic or anic the new supported catalysts
--silica-supported palladacycle or plex can be synthesized by the reaction of the hybrid materials with palladium the present dissertation,we have reported the synthesis,characterization of the new catalysts and their catalytic performances in
Heck catalysts show hi曲catalytic activity and addition,it can
be filtrated from the reaction mixture,SO it’S possible to recycle the catalyst.
and characterization ofSi02一supported palladacycle catalyst
(1).The immobilization of-N[-12 function group onto Si02 surface was investigated, silica-schiff base was prepared by o-Methoxybenzaldehyde grafting on amine functionalized silica,then a silica hybrid material supported plex has
been synthesized by the reaction ofsilica-schiffbase with Li2PdCh in methan01.
(2).Si02,Si02-NH2,silica-schiffbase,and the catalysts were characterized by FTIR, XRD,XPS,TG-DSC and the Elemental results showed t