反应详情

To a solution of 2-methylaniline (2.2 g, 20 mmol, purchased from TCI) in pyridine (1.7 ml. 1.7 g, 21.4 mmol) and DCM (85 ml), methanesulfonyl chloride (1.6 ml, 2.3 g, 20 mmol) was added dropwise over 10 minutes at 0° C. The reaction mixture was stirred at room temperature for 1 hour. After cooling to 0° C., aluminum trichloride (6.8 g, 51 mmol) was added to the reaction mixture carefully. Then acetyl chloride (1.9 g, 20 mmol) was added dropwise over 15 minutes. The reaction mixture was diluted with toluene (25 ml) and poured into 2 M HCl aqueous solution (500 ml) with stirring at 0° C. The precipitates were filtered, washed with water and dried in vacuo to afford the title compound (2.1 g, 43%) as yellow solids.

1. temperatureAfter cooling to 0° C.
2. stirringwith stirring at 0° C
3. filtrationThe precipitates were filtered
4. washwashed with water
5. customdried in vacuo