Propanedioic acid, monoethyl ester → Propanedioic acid, monoethyl ester

Participants

Reaction Steps

Using the procedure of Step C of Example 6, 1.34 g of magnesium and 8.8g of ethyl malonate were reacted to obtain ethoxy magnesium of ethyl malonate to which was added over 30 minutes at room temperature a solution of 12.4 g of the product of Step B in 10 ml of dry toluene. The mixture was held at room temperature for 45 minutes and was then poured into 50 ml of 2N hydrochloric acid and 50 ml of ice. The mixture was extracted with ether and the extracts were washed with 5% sodium bicarbonate solution and then with water until the wash water pH was 6. The extracts were dried over magnesium sulfate, treated with activated carbon and evaporated to obtain 18 g of ethyl 2-[1-(2-trifluoromethylphenylamino)-2-methyl-prop-1-ylidene]-propanedioate in the form of a yellow oil which was used as is for the next step.

Provenance & Evidence