反应详情

温度

60 °C

To a suspension of N-(3-(4-methoxypyridin-2-yl)phenyl)-N′-benzoylthiourea (429 mg) in methanol (5 ml) was added an aqueous sodium hydroxide solution (1N, 1.42 ml) dropwise. The mixture was stirred at 60° C. for 1 hour and cooled to ambient temperature. The pH was adjusted to 8.0 with 1N hydrochloric acid. The mixture was diluted with water (50 ml) and extracted with dichloromethane-methanol (4:1). The organic layer was washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was triturated with diisopropyl ether, collected by filtration, washed with diisopropyl ether and dried under reduced pressure to give N-(3-(4-methoxypyridin-2-yl)phenyl)thiourea (294 mg).

1. temperaturecooled to ambient temperature
2. extractionextracted with dichloromethane-methanol (4:1)
3. washThe organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated under reduced pressure
6. customThe residue was triturated with diisopropyl ether
7. filtrationcollected by filtration
8. washwashed with diisopropyl ether
9. customdried under reduced pressure