Simple exploration of Diethyl 2,2-bis(hydroxymethyl)malonate

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,20605-01-0, its application will become more common.

Reference of 20605-01-0 ,Some common heterocyclic compound, 20605-01-0, molecular formula is C9H16O6, 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.

EXAMPLE 1 (comparative example) Diethyl 1,5-dioxaspiro[5.5]undecane-3,3-dicarboxylate A stirred mixture of 165.0 g of diethyl bis(hydroxymethyl)malonate (98%, 0.75 mol), 75.3 g of cyclohexanone and 500 g of cyclohexane as a solvent and entrainer was admixed with 1.0 g of sulfuric acid. The mixture was then heated to reflux temperature (70-80 C.), the reaction water formed being continuously removed over a period of 5 hours. After the reaction was complete, the reaction mixture was cooled to room temperature and introduced into dilute, excess aqueous sodium hydrogen carbonate solution. The aqueous phase was re-extracted with methyl t-butyl ether, and the combined organic phases were washed once with water. After drying over sodium sulfate the solvents were distilled off on a rotary evaporator, and the product was isolated by distillation in an oil pump vacuum. This gave 168.4 g of target product (75% of the theoretical yield, based on the diethyl bis(hydroxymethyl)malonate used) with a boiling point of 140 C./0.2 mm. The purity, determined by gas chromatography, was 97 to 98 FID percent by area.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,20605-01-0, its application will become more common.

Reference:
Patent; Huels Aktiengesellschaft; US5932747; (1999); A;,
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