Reference of 10203-58-4,Some common heterocyclic compound, 10203-58-4, name is Diethyl isobutylmalonate, molecular formula is C11H20O4, 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.
(b) 2-(S-Acetylthiomethyl)4-methylpentanoic acid Hydrolysis of 91.1 g of isobutyldiethyl malonate is accomplished by digesting a solution of the ester in 300 ml of methanol and 400 ml of 10% NaOH for 6 hours at 80 C. The solution is concentrated in vacuo to 400 ml. It is acidified with 10% aqueous HCl and product is extracted with ethyl acetate to yield 67.6 g of the diacid. This crystallized on standing. M.P. 94-95 C. The diacid is suspended in 400 ml of water and cooled to 5 C. Aqueous 40% dimethylamine (50 g) and aqueous 37% formaldehyde (35.7 g) are added in that order. The solution is stirred overnight and Mannich base solid product is filtered and dried in vacuo to yield 57.3 g. M.P. 134-137 C. with CO2 and dimethylamine given off. The Mannich base (57.3 g) is suspended in 200 ml of water and 43 g of 50% NaOH in 100 ml of water is added until pH is 9. This solution is heated on the steam cone under nitrogen overnight. It is neutralized with 10% HCl and product is extracted with ethyl acetate to yield 23.8 g. The crude unsaturated acid is chromatographed (twice) on 200 g of silica to give 21.6 g of pure acid.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Diethyl isobutylmalonate, its application will become more common.
Reference:
Patent; E. R. Squibb & Sons, Inc.; US4382081; (1983); A;,
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