反应详情

While stirring under ice-cooling, 10% hexane solution of sulfuryl chloride (0.019 ml, 0.24 mmol) was added to acetic acid (3 ml) solution of 2-{2,5-bis(trifluoromethyl)phenyl}amino-3-ethyl-6-trifluoromethyl-4(3H)-pyrimidinone (0.10 g, 0.24 mmol), followed by stirring for 1.5 hours while gradually returning to room temperature. After completion of the reaction, ice-water (10 ml) and ether (10 ml) were added to the reaction solution to separate the organic layer, and the resulting aqueous layer was extracted with ether (10 ml×3). The organic layers were combined, washed with water (20 ml×2) and then dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the resulting filtrate was concentrated under a reduced pressure. By recrystallizing the thus obtained crude product from chloroform/hexane, 2-{2,5-bis(trifluoromethyl)phenyl}amino-5-chloro-3-ethyl-6-trifluoromethyl-4(3H)-pyrimidinone [Compound No. 49] was obtained.

1. temperaturecooling
2. stirringby stirring for 1.5 hours
3. customwhile gradually returning to room temperature
4. additionwere added to the reaction solution
5. customto separate the organic layer
6. extractionthe resulting aqueous layer was extracted with ether (10 ml×3)
7. washwashed with water (20 ml×2)
8. dry with materialdried over anhydrous magnesium sulfate
9. customThe drying agent was removed by filtration
10. concentrationthe resulting filtrate was concentrated under a reduced pressure
11. customBy recrystallizing the
12. customthus obtained crude product from chloroform/hexane