J. Min
2006
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Journal
Chemical Industry and Engineering Progress
Abstract
A process suitable for large-scale preparation of 3-amino-1H-pyrrole-2-carboxylate hydrochloride was developed.The title compound was synthesized through four steps,which include the condensation of ethyl formate with acetonitrile by using NaH as the promoter,condensation with diethyl 2-aminomalonate hydrochloride,cyclization in the presence of NaOEt,and reaction with hydrogen chloride.The characteristics of the title compound was investigated with 1HNMR and elemental analysis.The results showed that the optimum molar ratio of n(HCOOC2H5) ∶ n(CH3CN) ∶ n(NaH) ∶ n(NH2CH(COOC2H5)2HCl) was 1∶1.2∶1.3∶0.5,the reaction temperature was 20 ℃ and the reaction time was 24 and 48 hours respectively.The procedure was a suitable alternative to the traditional processes due to safety,stability,and handling concerns.