Hydrochloric Acid → HCID 178517435, compound

Participants

Reaction Steps

To 7.10 g of phenylmagnesium bromide (32% THF solution) was added dropwise a solution of 953 mg of 2-amino-3-chlorobenzonitrile in THF (7 ml) at room temperature, followed by heating under reflux for 30 minutes. To the resulting reaction product was added dropwise 885 mg of methyl chlorocarbonate under ice cooling, followed by heating under reflux for 40 minutes. The resulting reaction solution was cooled and poured into 40 ml of 2N-hydrochloric acid, and 8 g of sodium bicarbonate and 20 ml of MTBE were added thereto, followed by stirring. Then, precipitated crystals were collected by filtration to obtain 1.30 g of the titled compound. 1H NMR (DMSO-d6): 7.24(1H, t, J=8.0 Hz), 7.57-7.70 (6H, m), 7.90-7.93 (1H, m), 11.45 (1H,br. s).

Provenance & Evidence