反应详情

The reaction of 4.5 g (0.02 mole) of TNT with 4.6 g (0.01 mole) of 3-chloro-2,2',4,4',6,6'-hexanitrostilbene was carried out as in the above reactions. The crude reaction product, after extraction with methanol was a brittle mass which was dissolved in 50 mol of acetonitrile, diluted with an equal volume of methanol and heated on a hot plate with magnetic stirring. Light yellow crystals separated and were filtered off, washed well with methanol and dried. This material weighed 4.8 g, 71% of the theoretical yield, melted at 168°-170° (dec), and elemental analysis showed that it contained a mole of acetonitrile. Calcd for C23H12N10O18 : N, 19.6. Found: N, 19.7, 19.4. Recrystallized from 50 ml of THF with 50 ml of methanol added to the hot THF solution after filtering, the product separated in very fine, almost colorless crystals, mp 210°-211°C. Anal. Calcd for C21H9N9O18 : C, 37.2; H, 1.3; N, 18.8. Found: C, 37.5, 37.7; H, 1.6, 1.5; N, 19.0, 18.4.

1. customThe crude reaction product
2. extractionafter extraction with methanol
3. temperatureheated on a hot plate with magnetic stirring
4. customLight yellow crystals separated
5. filtrationwere filtered off
6. washwashed well with methanol
7. customdried
8. customRecrystallized from 50 ml of THF with 50 ml of methanol
9. additionadded to the hot THF solution
10. filtrationafter filtering
11. customthe product separated in very fine, almost colorless crystals, mp 210°-211°C