50826-00-1

99066-80-5

Methyl 3-methyl-3-carbamoyl-5-nitrobenzoate (30 mmol) was used as a starting material and dissolved in 1,2-dichloroethane (100 mL). POCl3 (33 mmol) was added to this solution and the reaction mixture was subsequently heated to reflux for 3 hours. After completion of the reaction, it was cooled to room temperature and the reaction solution was slowly poured into water. The organic layer was separated and washed sequentially with saturated NaHCO3 solution and brine. The organic layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford the target product methyl 3-cyano-5-nitrobenzoate in 90% yield.