反应详情

A suspension of 4-bromo-2-fluorobenzonitrile (25.0 g, 125 mmol) in IMS (88 mL) at 0-5° C. and treated dropwise with acetyl chloride (71 mL, 1 mol) maintaining the temperature below 10° C. The reaction vessel was sealed and the mixture stirred at RT for 18 h before concentrating in vacuo. The resultant residue was triturated in diethyl ether to give 4-Bromo-2-fluoro-benzimidic acid ethyl ester hydrochloride as a white solid (20.3 g, 57%). 1H NMR δ (ppm) (DMSO-d): 7.93-7.88 (1 H, m), 7.85-7.76 (1 H, m), 7.72-7.64 (1H, m), 4.60 (2 H, q, J=7.02 Hz), 1.47-1.38 (3 H, m).

1. temperaturemaintaining the temperature below 10° C
2. customThe reaction vessel was sealed
3. concentrationbefore concentrating in vacuo
4. customThe resultant residue was triturated in diethyl ether