ethyl hydrogen diethylmalonate synthesis

Yield:84930-02-9 23.1 g

Reaction Conditions:

with lithium hydroxide monohydrate;sodium hydroxide in methanol at 20;

Steps:

22-3.1

(1) To a solution of dimethyl diethylmalonate (25 g) in methanol (250 mL) was added a 1N aqueous sodiumhydroxide solution (132.8 mL), and the mixture was stirred at room temperature overnight. The methanol was distilledoff under reduced pressure, and the residue was washed with methylene chloride. To the aqueous layer was added 1Nhydrochloric acid to adjust the pH to 3, and the mixture was extracted with diethyl ether. The extract was washed withwater, dried over anhydrous magnesium sulfate. After drying, concentration under reduced pressure provided Compound2 (23.1 g) as a colorless oil.

References:

EP2862856,2015,A1 Location in patent:Paragraph 1289; 1290