反应详情

温度

-40 °C

Ethyl ethoxythiocarbonylcarbamate (1 molar proportion) was added to a stirred solution of potassium carbonate in water (10 ml. per gram of carbamate). After 15 minutes stirring, the solution was filtered and dimethyl sulphate added dropwise to the filtrate with vigorous stirring over 45 minutes. The mixture was then stirred for 1 hour and extracted with light petroleum. The extracts were dried and cooled to -40° C., when the carbamate separated. Recrystallised from petroleum, the carbamate had a melting point of 38°-39° C. (b) N,N-Dimethylguanidine hydrochloride (3.23 g; 0.026 mol.) was added to a solution of sodium (0.61 g; 0.026 mol.) in anhydrous ethanol (50 ml.) and the mixture was heated under reflux for 30 minutes. The carbamate prepared in (a) above (5.0 g., 0.026 mol.) was then added and the mixture heated under reflux for 22 hours. The ethanol was removed, water (75 ml.) added, and the pH of the solution adjusted to 6 to 7 with acetic acid. The product was collected, washed with water, and recrystallised from ethanol to give 4-dimethylamino-6-ethoxy-1,3,5-triazin-2-one.

1. filtrationthe solution was filtered
2. additiondimethyl sulphate added dropwise to the filtrate
3. stirringwith vigorous stirring over 45 minutes
4. stirringThe mixture was then stirred for 1 hour
5. extractionextracted with light petroleum
6. customThe extracts were dried
7. customwhen the carbamate separated
8. customRecrystallised from petroleum
9. temperaturethe mixture was heated
10. temperatureunder reflux for 30 minutes
11. additionwas then added
12. temperaturethe mixture heated
13. temperatureunder reflux for 22 hours
14. customThe ethanol was removed
15. additionwater (75 ml.) added
16. customThe product was collected
17. washwashed with water
18. customrecrystallised from ethanol