반응 #1687624

반응 방정식

hydrochloric acid

sodium carbonate

thiosemicarbazide

nicotinoyl chloride

→

3-Mercapto-5(3-pyridyl)-1,2,4-triazole

용매

water

pyridine

반응 조건

후처리

1. 1
   온도After reflux for 40 min. the reaction mixture
2. 2
   농축was concentrated to half the original volume, 500 ml of water
3. 3
   workup.ADDITIONwas added
4. 4
   기타stored in the cold overnight
5. 5
   기타formed
6. 6
   기타was removed by filtration
7. 7
   기타the filtrate was evaporated in vacuo
8. 8
   workup.DISSOLUTIONThe resulting heavy, yellow oil was dissolved in 300 ml of water
9. 9
   온도After reflux for 4 h the solution
10. 10
    온도was cooled
11. 11
    기타The formed, colorless precipitate, 65, was isolated by filtration
12. 12
    기타dried in vacuo

실험 절차

To a solution of 19 g (0.200 mol) of thiosemicarbazide in 175 ml of dry pyridine, 29 g (0.200 mol) of nicotinoyl chloride was slowly added at 10° C. After reflux for 40 min. the reaction mixture was concentrated to half the original volume, 500 ml of water was added, and stored in the cold overnight The precipitate formed was removed by filtration, and the filtrate was evaporated in vacuo. The resulting heavy, yellow oil was dissolved in 300 ml of water, and 64 g (0.600 mol) of sodium carbonate in 400 ml of water was added. After reflux for 4 h the solution was cooled and acidified with conc. hydrochloric acid to pH=4. The formed, colorless precipitate, 65, was isolated by filtration and dried in vacuo. Yield: 35 g (0.297 mol, 98%).

출처