Hydrochloric Acid → HCID 53787511, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 50.0 g of 2-chloro-5-[3,6-dihydro-3,4-dimethyl-2,6-dioxo-1(2H)-pyrimidinyl]-4-fluorobenzoic acid isopropyl ester and 25.4 g of copper(I) cyanide in 225 ml of dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone is heated for 2.5 hours at 195° C. under nitrogen. The mixture is then cooled to room temperature and 2 l of ethyl acetate are added. The mixture is then poured onto 1.31 of water and 300 ml of 32% hydrochloric acid, and the whole is stirred for 45 minutes at room temperature until two distinct layers have formed. The organic phase is removed, washed twice with 200 ml of water each time and dried over anhydrous sodium sulfate. Concentration by evaporation of the organic solution yields crystalline 2-cyano-5-[3,6-dihydro-3,4-dimethyl-2,6-dioxo-1(2H)-pyrimidinyl]-4-fluorobenzoic acid isopropyl ester, m.p. 188°-200° C.

Provenance & Evidence