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With N-chloro-succinimide In N,N-dimethyl-formamide at 20℃; for 21h;
47%
With N-chloro-succinimide In N,N-dimethyl-formamide at 25℃;
93.1
Step 1 2-Amino-4,5-dichlorobenzonitrile A 10 mL round bottom flask was charged with 2-amino-4-chlorobenzonitrile (0.2 g, 1.31 mmol), N-chlorosuccinimide (0.19 g, 1.44 mmol) and DMF (5 mL). The resulting mixture was stirred at 25° C. overnight. Reaction progress was monitored by TLC (EtOAc/Petroleum ether=1:10). Work-up: the reaction mixture was diluted with EtOAc (40 mL) and washed with brine (40 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel with a 1:10 EtOAc/Petroleum ether, to afford 170 mg (47%) of the product as white solid. 1H NMR (300 MHz, CDCl3) δ: 7.45 (s, 1H), 6.88 (s, 1H), 4.48 (br, 2H).
47%
With N-chloro-succinimide In N,N-dimethyl-formamide at 25℃;
93.1
A 10 mL round bottom flask was charged with 2-amino-4- chlorobenzonitrile (0.2 g, 1.31 mmol), N-chlorosuccinimide (0.19 g, 1.44 mmol) and DMF (5 mL). The resulting mixture was stirred at 25 °C overnight. Reaction progress was monitored by TLC (EtO Ac/Petroleum ether = 1 : 10). Work-up: the reaction mixture was diluted with EtO Ac (40 mL) and washed with brine (40 mL). The organic layer was dried over anhydrous Na2SC>4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel with a 1 : 10EtOAc/Petroleum ether, to afford 170 mg (47%) of the product as white solid. NMR (300 MHz, CDC13) δ: 7.45 (s, 1H), 6.88 (s, 1H), 4.48 (br, 2H).
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