An efficient one‐pot synthesis method for multiple heterocyclic scaffolds was carried out based on the cyano‐containing amphiphilic Claisen‐Schmidt reaction intermediate. Several valuable heterocyclic compounds including isoindolinone, flavonoid and isobenzofuranone were conveniently synthesized from o‐cyanobenzaldehyde and o‐hydroxyacetophenone by controlling the reaction temperature, catalyst and solvent. In addition, a density functional theory (DFT) based calculation was carried out on the key amphiphilic intermediate for understanding the reaction selectivity in water and non‐aqueous solution.
In this paper, the prenyl alcohol was catalyzed synthesized in anhydrous system by using isoprene and dichloroacetic acid as raw material and sodium dichloroacetate as catalyst. The obtained product was mainly characterized by FT-IR and GC. Furthermore, the olefine acid ratio, reaction time, amount of catalyst, saponification time and NaOH concentration were systematically investigated during the work. The optimum reaction conditions are as follows: the olefine acid ratio was 1:2, reaction time was 2h, amount of catalyst was 1.8g, saponification time was 2h and NaOH concentration was 4mol/L, the yield of prenyl alcohol was 45%.
The improved synthesis of 3, 3-dimethyl-4-pentenoic acid methyl ester (DPE) had been discovered. In new process, orthophosphate (85%) and sodium methoxide(98%)was used as catalysts at different stages of the reaction, the amount of azeotropic mixture of DPE and the byproduct 3'-methyl-2'-butenyl-3, 3-dimethyl-pentenpate (MBDP) is reduced, the recovery rate of product DPE is improved. under the optimal reaction condition, the highest yield of DPE approach 84%. Improved the process is more suitable for industrial production.
The new process of 1-(3,4-dichloropheny)-3-methyl-pyrazolone-5-one (34DCPMP) synthesis had been discovered, which using 3,4-dichloro phenylhydrazine hydrochloride(DCPH) and ethyl acetoacetate as the raw material , The product was obtained by the route during cyclization in aqueous medium. The structure of products was confirmed by 1HNMR, 13CNMR and IR. The effects of factors on the yield of products were investigated. It was found that the yield of 34DCPMP can reach 98.7% under the optimal reaction condition of n(34DCPH):n(ethyl acetoacetate) with 1:1.1, n(34DCPH):n(Na2SO3) with 1.3:1 at 80°C, and pH 7.5 for 3h. The chromatographic purity can be higher than 98.2%.
In this paper, the prenyl alcohol was catalyzed synthesized by using isoprene and dichloroacetic acid as raw material and sodium dichloroacetate as catalyst. The obtained product was mainly characterized by FT-IR and GC. Furthermore, the olefine acid ratio, reaction time, amount of catalyst, saponification time, NaOH concentration and distilled water consumption were systematically investigated during the work. The optimum reaction conditions were as follows: the olefine acid ratio was 1:2, reaction time was 2h, amount of catalyst was 1.5g, saponification time was 2h, NaOH concentration was 4mol/L and amount of distilled water was 0.2mL, the yield of prenyl alcohol was 26%
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