Sodium hydride → HCID 19896204, compound

Participants

Reaction Conditions

Reaction Steps

8.7 g of ethyl 3-amino-3-(2-chlorophenyl)-2-propenoate was added dropwise to a 40 ml dimethylformamide of 1.8 g of sodium hydride (purity: 55%) with stirring at 0° C. The solution was stirred at room temperature for 15 minutes, cooled to 0° C. and added dropwise with a 20 ml dimethylformamide solution of 7.2 g of ethyl 4-methoxymethoxyphenylcarbamate. After stirring the solution at 120° C. for 2 hours, the solvent was distilled away under reduced pressure. The residue was dissolved with 200 ml of water and washed with diethyl ether. The obtained aqueous layer was added into a mixed solution of 50 ml of concentrated hydrochloric acid and 150 g of ice. The precipitated crystals were filtered out and dried under reduced pressure to obtain 10.0 g of 3-(4-methoxymethoxyphenyl)-6-(2-chlorophenyl)-2,4(1H,3H)-pyrimidinedione.

Provenance & Evidence