反応 #1687624

反応方程式

hydrochloric acid

sodium carbonate

thiosemicarbazide

nicotinoyl chloride

→

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

溶媒

water

pyridine

反応条件

後処理

1. 1
   温度After reflux for 40 min. the reaction mixture
2. 2
   濃縮was concentrated to half the original volume, 500 ml of water
3. 3
   workup.ADDITIONwas added
4. 4
   その他stored in the cold overnight
5. 5
   その他formed
6. 6
   その他was removed by filtration
7. 7
   その他the filtrate was evaporated in vacuo
8. 8
   workup.DISSOLUTIONThe resulting heavy, yellow oil was dissolved in 300 ml of water
9. 9
   温度After reflux for 4 h the solution
10. 10
    温度was cooled
11. 11
    その他The formed, colorless precipitate, 65, was isolated by filtration
12. 12
    その他dried in vacuo

実験手順

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%).

出典