反应详情

60 g of 3-mercapto-1,2,4-triazolo(4,3-a)pyridine are dissolved in 500 ml of ethanol. 21 g of sodium carbonate and 29 ml of 2-bromoethanol are then added. The reaction mixture is heated under reflux for 9 hours, the mineral substances are filtered off, the filtrate is then concentrated in vacuo, the concentrate is taken up with water acidified with 0.5N hydrochloric acid and extraction is carried out with chloroform. The aqueous phase is then rendered basic with aqueous ammonia, saturated with sodium chloride and then extracted with chloroform. The chloroform phase obtained is dried over magnesium sulfate and then concentrated in vacuo. The crystals which then form are taken up with pentane, filtered off, washed with pentane and dried to give 69.2 g of 2-[1,2,4-triazolo(4,3-a)pyridin-3-ylmercapto]ethanol in the form of crystals melting at 84° C.

1. temperatureThe reaction mixture is heated
2. temperatureunder reflux for 9 hours
3. filtrationthe mineral substances are filtered off
4. concentrationthe filtrate is then concentrated in vacuo
5. extractionacidified with 0.5N hydrochloric acid and extraction
6. extractionextracted with chloroform
7. customThe chloroform phase obtained
8. dry with materialis dried over magnesium sulfate
9. concentrationconcentrated in vacuo
10. customThe crystals which then form
11. filtrationfiltered off
12. washwashed with pentane
13. customdried