反应详情

To a stirred solution of 5.0 g. (0.015 mole) of N-(dimethylamino)-3-chloro-2,6-dinitro-4-trifluoromethylaniline and 50 ml. of anhydrous methanol was added 3.77 g. (0.015 mole) of a 21.8% methanolic sodium methoxide solution. The resultant mixture was stirred at room temperature for 6 hours and was then refluxed overnight for 16 hours. The methanol was then evaporated under vacuum leaving a yellow-solid residue. To the residue was added 150 ml. of water and the mixture stirred for 30 minutes to dissolve the NaCl and any other water-soluble materials. The mixture was then filtered and the water-insoluble solids were washed well with water. The solids were then dissolved in 30 ml. of refluxing 95% ethanol. On cooling, the product crystallized and was isolated by filtration to give 3.83 g. (77.7%) of a yellow crystalline solid; m.p. 109°-110.5° C. After recrystallization from 95% ethanol, the product melts at 110°-111.5° C.

1. temperaturewas then refluxed overnight for 16 hours
2. customThe methanol was then evaporated under vacuum
3. customleaving a yellow-solid residue
4. additionTo the residue was added 150 ml
5. filtrationThe mixture was then filtered
6. washthe water-insoluble solids were washed well with water
7. dissolutionThe solids were then dissolved in 30 ml
8. temperatureof refluxing 95% ethanol
9. temperatureOn cooling
10. customthe product crystallized
11. customwas isolated by filtration
12. customto give 3.83 g
13. customAfter recrystallization from 95% ethanol