These common heterocyclic compound, 105-53-3, name is Diethyl malonate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 105-53-3
EXAMPLE 14: PREPARATION OF 1 ,1 CYCLOPRANEDIESTER (FORMULA XVI):1 ,2-dichloroethane (400 liters), diethyl malonate (145 kg), N,N-dimethyl formamide (365 liters), and potassium carbonate (187 kg) were taken into a reactor equipped with a Dean-Stark type azeoptropic apparatus. The reaction mixture was heated to reflux followed by stirring for about 30 hours, simultaneously removing unwanted water that was collected in the Dean Stark apparatus. The reaction mixture was cooled to about 30 0C. The reaction mass was filtered and the filter washed with 510 L of 1 ,2-dichloroethane. The obtained organic layer was washed with water (4*510 L water) and distilled completely under vacuum below 6O0C to obtain a residue. The obtained residue was cooled to 35 0C and high vacuum applied. The reaction mass was heated slowly below 75C and collect the first fraction. The second fraction was collected by maintaining the temperature at 900C and the third fraction was collected by maintaining the temperature below 120C for about 5 hours to afford 18.5 kg (2nd and 3rd fractions) of the title compound. Purity by GC: 92.44%.
The synthetic route of Diethyl malonate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; DR. REDDY’S LABORTORIES, LTD.; DR. REDDY’S LABORATORIES, INC.; WO2008/58118; (2008); A2;,
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