反应详情

温度

65 °C

Ethyl 2,3-dibromobutyrate (1.33 g, 48.5 mmol) was added dropwise over 15 minutes to a solution of 10 g (49 mmol) of 3-amino-5-benzylthio-1,2,4-triazole in 20 ml of pyridine heated to 65° C. After the addition was complete, the reaction mixture was heated at 65° C. for 20 hours, cooled to room temperature and filtered. The filtrate was concentrated by evaporation at reduced pressure. The residue was triturated with methanol to separate 1.64 g (13%) of the desired product as a colorless crystalline solid, m.p. 219°-220° C. IR and 1H NMR spectra were in agreement with the assigned structure.

1. additionAfter the addition
2. temperaturethe reaction mixture was heated at 65° C. for 20 hours
3. temperaturecooled to room temperature
4. filtrationfiltered
5. concentrationThe filtrate was concentrated by evaporation at reduced pressure
6. customThe residue was triturated with methanol
7. customto separate 1.64 g (13%) of the desired product as a colorless crystalline solid, m.p. 219°-220° C