反应详情

温度

120 °C

In 20 ml of DMF was dissolved 1.20 g of N-[2-(2-cyanophenylthio)phenyl]-4-hexyloxybenzamide followed by addition of 0.36 g of sodium azide and 0.30 g of ammonium chloride, and the mixture was stirred at 120° C. for 3 hours. Then, the same amounts of sodium azide and ammonium chloride as above were added twice at an interval of 3 hours. The reaction mixture was then acidified with diluted hydrochloric acid and the resulting crystals were collected by filtration and washed with water. The crystals were dissolved in chloroform and dried over magnesium sulfate and the solvent was distilled off. The crystals thus obtained were recrystallized from ethyl acetate-n-hexane to give 1.1 g of the title compound as white crystals, m.p. 154°-156° C.

1. filtrationthe resulting crystals were collected by filtration
2. washwashed with water
3. dissolutionThe crystals were dissolved in chloroform
4. dry with materialdried over magnesium sulfate
5. distillationthe solvent was distilled off
6. customThe crystals thus obtained
7. customwere recrystallized from ethyl acetate-n-hexane