反应详情

To a solution of hydrazine monohydrate (9.66 g) in ethanol (100 ml), ethyl glycolate (20.09 g) was slowly added dropwise with keeping the reaction temperature under 10° C. at room temperature. The mixture was stirred at room temperature for 4 hours, propyl isothiocyanate (20 ml) was slowly added dropwise thereto with keeping the reaction temperature under 10° C. The mixture was stirred for 64 hours at 40° C., cooled to room temperature, and ice-water (50 ml) was added to the mixture. The mixture was stirred for 15 miuntes, 5N aqueous solution of sodium hydroxide (40 ml) was added to the mixture, and the mixture was stirred for 4 hours at 60°. Concentrated hydrochloric acid was added dropwise to the solution at 0° C. to adjust pH to 6, and the precipitated crystals were removed by filtration. The mixture was concentrated under reduced pressure, and the precipitated crystals were collected by filtration. The crystals were washed with water, to give 3-hydroxymethyl-5-mercapto-4-propyl-4H-1,2,4-triazole (23.45 g) as colorless crystals.

1. customunder 10° C.
2. customat room temperature
3. customunder 10° C
4. stirringThe mixture was stirred for 64 hours at 40° C.
5. temperaturecooled to room temperature
6. additionwas added to the mixture
7. stirringthe mixture was stirred for 4 hours at 60°
8. customthe precipitated crystals were removed by filtration
9. concentrationThe mixture was concentrated under reduced pressure
10. filtrationthe precipitated crystals were collected by filtration
11. washThe crystals were washed with water