反应详情

4.31 g of 1-(2-biphenylylsulfonyl) 3-(4,6-dimethoxy-1,3,5-triazin-2-yl)thiourea were suspended in 50 ml of dry acetonitrile, and a solution of 0.3 g of metallic sodium in 10 ml of ethanol was added to the suspension, and the mixture was heated under reflux for 30 minutes. After cooling, 1.85 g of methyl iodide were added, and the mixture was heated under reflux for 5 hours. After cooling, the reaction mixture was poured into 100 ml of water, and extracted with methylene chloride. Methylene chloride was distilled off under reduced pressure from the extract, and the residue was recrystallized from ethanol to give 2.1 g of 1-(2-biphenylylsulfonyl) 3-(4,6-dimethoxy-1,3,5-triazin-2-yl) 2-methylisothiourea represented by the following formula: ##STR29##

1. temperaturethe mixture was heated
2. temperatureunder reflux for 30 minutes
3. temperatureAfter cooling
4. temperaturethe mixture was heated
5. temperatureunder reflux for 5 hours
6. temperatureAfter cooling
7. extractionextracted with methylene chloride
8. distillationMethylene chloride was distilled off under reduced pressure from the extract
9. customthe residue was recrystallized from ethanol