反応 #473473

反応方程式

2-amino-4-chlorobenzonitrile

pyridine

PhCOCl

→

title compound

N-(5-Chloro-2-cyanophenyl)benzamide

溶媒

DCM

反応条件

後処理

1. 1
   洗浄The reaction mixture was washed (H2O, 2 M aq HCl (2×), H2O, brine)
2. 2
   乾燥dried (Na2SO4)
3. 3
   濃縮concentrated under reduced pressure

実験手順

To a solution of 2-amino-4-chlorobenzonitrile (7.25 g, 47.5 mmol), in anh. pyridine (38 mL, 475 mmol) and DCM (300 mL) cooled in an ice-H2O bath under Ar was added PhCOCl (5.8 mL, 50 mmol) dropwise. The reaction was allowed to slowly warm to rt within the cooling bath and then was stirred at rt overnight. The reaction mixture was washed (H2O, 2 M aq HCl (2×), H2O, brine), dried (Na2SO4) and concentrated under reduced pressure to afford the title compound as a white solid; MS (ES+): m/z 257.1 (100) [MH+]; HPLC: tR=3.27 min (OpenLynx, polar—5 min).

出典