反应详情

温度

25 °C

A mixture of 2-chloro-5-nitrobenzoic acid (15.0 g, 74.0 mmol) and 200 mL of dichloromethane was reacted with oxalyl chloride (16.2 mL, 186.0 mmol) and a catalytic amount of dimethylformamide. The mixture was stirred at 25° C. for 3 hours. The solvent was removed in vacuo, and the residue was redissolved in 200 mL of dichloromethane. The solution was cooled to 0° C., and ammonia was bubbled through the cold solution for 5 minutes, whereupon the product precipitated to form solution. The product was collected by filtration to yield 6.8 g, mp 174°-175° C.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was redissolved in 200 mL of dichloromethane
3. temperatureThe solution was cooled to 0° C.
4. customammonia was bubbled through the cold solution for 5 minutes, whereupon the product
5. customprecipitated
6. customto form solution
7. filtrationThe product was collected by filtration
8. customto yield 6.8 g, mp 174°-175° C.