Synthesis of New Medicine Intermediate 2-Amino-4-hydroxy-3-methoxybenzaldehyde
Wang Tian-yi
Abstract
Wang Tian-yi
Abstract
A new medical intermediate 2-amino-4-hydroxy-3-methoxy benzaldehyde,was synthesized from vanillin via desertification,nitration,reduction and hydrolyzation.The effect of reaction time,reaction temperature and hydrochloric acid adding time were investigated through single experiment and orthogonal experiment.The optimal conditions were as followed: the reaction time was 1.75 h,the reaction temperature was 30℃ and the hydrochloric acid adding time was 15 min after pulverized iron being added.The steady yield of reduction was 88.08% and the total yield was 56.04%.The new compound 2-amino-4-acetoxy-3-methoxy-benzaldehyde was in that process;the structure was confirmed by IR.The structure of final product was confirmed by 1H NMR.There were many medical intermediate synthesized during this routing.
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A new medical intermediate 2-amino-4-hydroxy-3-methoxy benzaldehyde,was synthesized from vanillin via desertification,nitration,reduction and hydrolyzation.The effect of reaction time,reaction temperature and hydrochloric acid adding time were investigated through single experiment and orthogonal experiment.The optimal conditions were as followed: the reaction time was 1.75 h,the reaction temperature was 30℃ and the hydrochloric acid adding time was 15 min after pulverized iron being added.The steady yield of reduction was 88.08% and the total yield was 56.04%.The new compound 2-amino-4-acetoxy-3-methoxy-benzaldehyde was in that process;the structure was confirmed by IR.The structure of final product was confirmed by 1H NMR.There were many medical intermediate synthesized during this routing.
Key concepts: Benzaldehyde, Hydrochloric acid, Yield (engineering), Chemistry, Hydrolysis, Vanillin, Nitration, Fourier transform infrared spectroscopy