Study on the synthesis of 2,2′-diaminodibenzyl
Feng Xiao-qing
Abstract
Feng Xiao-qing
Abstract
o-Nitrobenzyl chloride was reduced to prepare 2,2′-diaminodibenzyl.The experimental conditions,such as materials ratio,reaction temperature and reaction time were investigated.Results showed that the optimal condition for condensation reaction were found as:n(o-nitrobenzyl chloride)∶n(Na) =1∶2,reflux time 7 h,under which the yield of 2,2′-dinitrodibenzyl was 85% based on o-nitrobenzyl chloride and the purity was 97.32% as determined by HPLC;proper reduction reaction conditions were found as:n(2,2′-dinitrodibenzyl)∶n(Fe)=1∶7,H2O and C2H5OH as solvent,V(H2O)∶V(C2H5OH) =2∶1,reaction temperature 90 ℃,reaction time 4 h,under which the yield of 2,2′-diaminodibenzyl was 97.5% based on 2,2′-dinitrodibenzyl and the purity was 98.86% as determined by HPLC.The molecular structures of product were identified by 1H NMR,13C NMR and LC-MS.
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o-Nitrobenzyl chloride was reduced to prepare 2,2′-diaminodibenzyl.The experimental conditions,such as materials ratio,reaction temperature and reaction time were investigated.Results showed that the optimal condition for condensation reaction were found as:n(o-nitrobenzyl chloride)∶n(Na) =1∶2,reflux time 7 h,under which the yield of 2,2′-dinitrodibenzyl was 85% based on o-nitrobenzyl chloride and the purity was 97.32% as determined by HPLC;proper reduction reaction conditions were found as:n(2,2′-dinitrodibenzyl)∶n(Fe)=1∶7,H2O and C2H5OH as solvent,V(H2O)∶V(C2H5OH) =2∶1,reaction temperature 90 ℃,reaction time 4 h,under which the yield of 2,2′-diaminodibenzyl was 97.5% based on 2,2′-dinitrodibenzyl and the purity was 98.86% as determined by HPLC.The molecular structures of product were identified by 1H NMR,13C NMR and LC-MS.
Key concepts: Yield (engineering), Chemistry, High-performance liquid chromatography, Chloride, Solvent, Reaction conditions, Condensation, Nuclear chemistry