反应详情

A solution of sodium nitrite (0.52 g, 7.57 mmol) in water (3 mL) was added dropwise to a cold (0° C.) mixture of 4-amino-3-methylbenzonitrile (1 g, 7.57 mmol) and concentrated HCl (12 mL) keeping the internal temperature below 0° C. After 5 min stirring, tin dichloride dihydrate (3.75 g, 16.6 mmol) in concentrated HCl (4 mL) was added at 0° C. The reaction mixture was allowed to warm to rt and stirred for 2 h. The resulting precipitate was collected by vacuum filtration and dried to provide 500 mg of the title compound. tR: 0.24 min (LC-MS 2); ESI-MS: 148 [M+H]+ (LC-MS 2).

1. customthe internal temperature below 0° C
2. stirringstirred for 2 h
3. filtrationThe resulting precipitate was collected by vacuum filtration
4. customdried