反应详情

Ethoxyacetyl chloride (57 g) was added slowly to a stirred solution of 4-methylthiosemicarbazide (53.5 g) in dry pyridine (500 ml) at 0°-5°. The mixture was allowed to attain room temperature and stirring was continued for 18 hours. Following concentration under reduced pressure the residue was treated with a solution of sodium (21.4 g) in ethanol (500 ml) and the mixture was heated under reflux for 24 hours. Following concentration and acidification with hydrochloric acid a solid was obtained. After partial concentration the solid was collected and recrystallised from ethyl acetate to give 3-ethoxymethyl-4-methyl-1,2,4-triazoline-5-thione (53 g) m.p. 137°-138°.

1. customto attain room temperature
2. concentrationconcentration under reduced pressure the residue
3. additionwas treated with a solution of sodium (21.4 g) in ethanol (500 ml)
4. temperaturethe mixture was heated
5. temperatureunder reflux for 24 hours
6. concentrationconcentration and acidification with hydrochloric acid a solid
7. customwas obtained
8. concentrationAfter partial concentration the solid
9. customwas collected
10. customrecrystallised from ethyl acetate