反应详情

A 10 g sample of 2-chloro-3-nitropyridine, an 8 g sample of potassium isothiocyanate, and 75 ml of acetic acid were combined and refluxed for 2 h. The reaction mixture was then cooled and poured into 400 ml of ice/H2O. The resulting solid was washed with water, redissolved in ethyl acetate and washed (4×) with water. The ethyl acetate solution was then treated with activated carbon, dried over anhydrous Na2SO4, filtered and evaporated to dryness to provide 3.72 g of the title compound. m.p.=115°-118° C.

1. temperaturerefluxed for 2 h
2. temperatureThe reaction mixture was then cooled
3. washThe resulting solid was washed with water
4. dissolutionredissolved in ethyl acetate
5. washwashed (4×) with water
6. additionThe ethyl acetate solution was then treated with activated carbon
7. dry with materialdried over anhydrous Na2SO4
8. filtrationfiltered
9. customevaporated to dryness