Modern Organic Chemistry Research

Download PDF (334.8 KB) PP. 24 - 29 Pub. Date: November 17, 2016

DOI: 10.22606/mocr.2016.11003

• Xiu-yan Pang^*
  College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China
• Xiu-zhu Shi
  College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China

In the synthesis of diethyl malonate with ethanol and malonic acid as reactants, the catalytic activity of expandable graphite (EG) was investigated, which was prepared by simple and rapid method with natural flake graphite, potassium permanganate and sulfuric acid (75%) as per the mass ratio of 1.0:0.15:6.67. The ethanol to acid mole ratio, EG dosage and its repetitive effectiveness were determined through single factor experiments. Appropriate condition for the synthesis of diethyl malonate was determined as: ethanol to malonic acid mole ratio was 6.0:1.0, EG was added as per an 8% mass percentage of the total quality of reactants, cyclohexane was added at a level of 20 mL, the reaction maintained slight boiling state until no water separated. Under the above condition, yield of diethyl malonate reached 77.6%. Repetition experiments showed that the catalyst could be reused three times without obvious loss of activity. However, it was significantly reduced in the 4th time. Nevertheless, its expansion performance almost remained unchanged.

Sulfuric acid, expandable graphite, diethyl malonate, reutilization, catalytic activity.

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