反应详情

10 g (0.034 mol) 4-Iodo-3-nitrobenzoic acid (Compound VI-1) and 50 ml N,N-dimethylformamide were added into a reaction flask, stirred to dissolve, and cooled to below 10° C., and 7.5 ml (0.10 mol) sulfoxide chloride was added. After completion of the dropwise addition, the mixture was warmed to room temperature and reacted for one hour. The reaction mixture was poured into 200 ml aqueous solution of 30% methylamine with low temperature, stirred for 5 minutes to precipitate a solid, and then the mixture was added with 500 ml ice-water, stirred for 10 minutes, filtered. The solid was washed with water and dried to obtain N-methyl-4-iodo-3-nitrobenzamide (Compound VII-1), 6.5 g (0.021 mol), yield 62.3%.

1. dissolutionto dissolve
2. temperaturecooled to below 10° C.
3. additionAfter completion of the dropwise addition
4. customreacted for one hour
5. stirringstirred for 5 minutes
6. customto precipitate a solid
7. additionthe mixture was added with 500 ml ice-water
8. stirringstirred for 10 minutes
9. filtrationfiltered
10. washThe solid was washed with water
11. customdried