摘要
以卤化钯(X=Cl、Br、I)为原料,乙腈为溶剂,与1,2-二(二苯基膦)乙烷反应,合成了1,2-二(二苯基膦)乙烷卤化钯[Pd(dppe)X_2,dppe=1,2-二(二苯基膦)乙烷],产率均高于96%,其结构经~1H NMR,XRD和元素分析确证。以Suzuki反应和Stille C—C偶联反应为模板反应,研究了Pd(dppe)Cl_2的催化活性。结果表明:Pd(dppe)Cl_2对2-氯噻吩和对甲氧基苯硼酸的Suzuki偶联反应、4,7-二氯苯并噻二唑核或其他含苯并噻二唑核的卤代芳烃与其他芳香核的锡试剂的Stille C—C偶联反应的催化转化率分别为80%~85%和52%~60%,催化活性优于四(三苯基膦)钯(70%~85%和43%~50%)。
1,2-Bis ( diphenylphosphino ) ethane halogenated palladium ( II ) [ Pd ( dppe ) X2, dppe = 1,2- bis(diphenylphosphino) ethane- were synthesized with yield above 96%, using palladium chloride, acetonitrile and 1,2-bis(diphenylphosphino) ethane as the raw material. The structure was confimled by ^1H NMtl, XtlD and elemental analysis. The Suzuki and Stille C-C coupling reaction was used as a model reaction to evaluate the catalytic activities of Pd (dppe) C12. The results showed that the catalytic conversion rate of Pd (dppe) C12 for Suzuki coupling reaction of 2-chlorothiophene and pmethoxy-phenylboronic acid, Stille C-C coupling reaction of 4,7-dichlorobenzothiadiazole nucleus or other benzotriazole nucleus-containing halogenated aromatics and other aromatic nucleus tin reagents were about 80% - 85% and 52% - 60% , better and 43% -50%) tetrakis ( triphenylphosphine ) palladium (70% - 85 %
作者
张阳阳
巨少英
左川
沈善问
叶青松
余娟
ZHANG Yang-yang;JU Shao-ying;ZUO Chuan;SHEN Shan-wen;YE Qing-song;YU Juan(State Key Lab of Advanced Technologiesfor Platinum Metals,Kunming Institute of Precious Metals,Kunming 650106,China)
出处
《合成化学》
CAS
CSCD
北大核心
2018年第10期738-743,共6页
Chinese Journal of Synthetic Chemistry
基金
云南省科技厅项目"2800公斤/年新型铂族金属催化前驱体批量制备关键技术开发及产业化"(2015AA06)
关键词
1
2-二(二苯基膦)乙烷氯化钯
合成
晶体结构
催化活性
1,2-bis(diphenylphosphino)ethane dichloropalladium
synthesis
crystal structure
catalytic activity