反应详情

23.5 g (0.15 mol) of N-methyl-4-nitroaniline are dissolved in 400 ml of dioxane and combined with 22.2 g (0.3 mol) of lithium carbonate. Then 32.2 g (0.18 mol) of bromoacetylbromide are added dropwise in such a way that the internal temperature does not exceed 33° C. After 18 hours' stirring the reaction solution is evaporated down to 100 ml, combined with 500 ml of water and stirred for 1 hour. The precipitate formed is suction filtered, washed with water and dried. The crude product is stirred in 400 ml of ethyl acetate at 40° C. Then the insoluble matter is filtered off, the solution is evaporated down and the solid residue is triturated with ether.

1. customdoes not exceed 33° C
2. customis evaporated down to 100 ml
3. stirringstirred for 1 hour
4. customThe precipitate formed
5. filtrationfiltered
6. washwashed with water
7. customdried
8. stirringThe crude product is stirred in 400 ml of ethyl acetate at 40° C
9. filtrationThen the insoluble matter is filtered off
10. customthe solution is evaporated down
11. customthe solid residue is triturated with ether