摘要
采用"两步法",以吡咯和3,4-二甲基苯甲醛为原料,合成了四(3,4-二甲基苯基)卟啉(TDMPP,1);1与四水醋酸钴经络合反应合成四(3,4-二甲基苯基)卟啉钴(TDMPPCo,2),其结构经1H NMR,IR和荧光光谱确证。考察了金属盐的预处理、反应物浓度、浓缩比和投料比对合成2的收率影响。实验结果表明:在最佳反应条件[γ=n(1)∶n(四水乙酸钴)=1∶7,c(1)为22.95 mmol·L-1,回流(150℃)反应4 h,浓缩比η为75%]下,收率可达82%。
Tetra (3,4-dimethylphenyl) porphyrin ( TDMPP, 1 ) was synthesized by a two-step method using pyrrole and 3,4-dimethylbenzaldehyde as starting materials. Tetra (3,4-dimethylphenyl) por- phyrin cobalt (TDMPPCo, 2) was synthesized by complexation reaction of cobalt (II) acetate tetra- hydrate with 1. The structure was confirmed by 1H NMR, IR and fluorescence'spectra. Effects of met- al salt pretreatment, reactant concentration, concentration ratio and feed ratio on the yield of 2 were in- vestigated. The results showed that under the optimum conditions [ y = n (1) : n ( cobalt (II) acetate tet- rahydrate) = 1 : 7, c(1) was 22.95 mmol· L-1 , at 150℃ for 4 h, concentration ratio 7/was 75% ], the yield was up to 82%.
出处
《合成化学》
CAS
CSCD
2016年第12期1066-1070,共5页
Chinese Journal of Synthetic Chemistry
关键词
吡咯
四(3
4-二甲基苯基)卟啉钴
合成
光谱性质
pyrrole
tetra (3,4-dimethyl-phenyl) porphyrin-cobah
synthesis
spectroscopic property