反应详情

温度

100 °C

A glass reaction tube was charged with 4.0 grams (0.0108 mole) of N,N-di-n-propyl-3-chloro-2,6-dinitro-4-trifluoromethylaniline, 5.82 grams (0.0237 mole) of 6.95% ethanolic ammonia and 35 ml. of ethanol. The tube was sealed and heated in an oven at 100°C. for 68 hours. The contents of the tube were cooled and the ethanol removed by evaporation. Water was added to the solid orange rsidue to dissolve the ammnium chloride and the insoluble produced was separated by filtration. The product was dissolved in refluxing 95% ethanol. Upon cooling, orange needles and a yellow powder crystallized. The yellow powder was identified as 2,4-dinitro-6-trifluoromethyl-1,3-phenylenediamine and was separated from the desired product by filtration after extracting with boiling hexane. The desired product dissolved in the hexane and was isolated from the filtrate by evaporation of the hexane. The residue was recyrstallized from 95% ethanol to give orange needles, m.p. 124° - 125°C.

1. customA glass reaction tube
2. customThe tube was sealed
3. temperatureThe contents of the tube were cooled
4. customthe ethanol removed by evaporation
5. additionWater was added to the solid orange rsidue
6. dissolutionto dissolve the ammnium chloride
7. customthe insoluble produced
8. customwas separated by filtration
9. dissolutionThe product was dissolved
10. temperaturein refluxing 95% ethanol
11. temperatureUpon cooling
12. customorange needles and a yellow powder crystallized
13. customwas separated from the desired product by filtration
14. extractionafter extracting with boiling hexane
15. dissolutionThe desired product dissolved in the hexane
16. customwas isolated from the filtrate by evaporation of the hexane
17. customto give orange needles, m.p. 124° - 125°C.