反应详情

3.98 g of 1-(2-biphenylylsulfonyl)3-(4,6-dimethylpyrimidin-2-yl)thiourea was suspended in 50 ml of dry acetonitrile, and a solution of 0.3 g of metallic sodium in 10 ml of ethanol was added, and the mixture was heated under reflux for 30 minutes. After cooling, 1.85 g of methyl iodide was added, and the mixture was heated under reflux for 5 hours. The reaction mixture was cooled, and then poured into 100 ml of water. The product was extracted with methylene chloride. Methylene chloride was evaporated under reduced pressure, and the residue was recrystallized from ethanol to give 1.6 g of the desired 1-(2-biphenylylsulfonyl)3-(4,6-dimethylpyrimidin-2-yl)2-methylisothiourea (compound No. II-1) which was the same as obtained in Example 1. mp. 154°-157° C.

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. temperatureThe reaction mixture was cooled
7. extractionThe product was extracted with methylene chloride
8. customMethylene chloride was evaporated under reduced pressure
9. customthe residue was recrystallized from ethanol