反应详情

A mixture of N-[3-(dimethylamino)propyl]-N′-phenylthiourea (800 mg) obtained in Reference Example 3 as described below and 2-bromo-4′-bromoacetophenone (1.09 g) in ethanol (30 ml) was heated with reflux under nitrogen atmosphere. Nine hours thereafter, the reaction mixture was concentrated under reduced pressure, and to the residue was added a saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with chloroform. The organic layer was washed with a saturated brine, dried over sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform: methanol (50:1)), and crystallized from isopropyl alcohol to give the title compound (830 mg)

1. customobtained in Reference Example 3
2. temperaturewas heated
3. temperaturewith reflux under nitrogen atmosphere
4. concentrationNine hours thereafter, the reaction mixture was concentrated under reduced pressure
5. additionto the residue was added a saturated aqueous sodium hydrogen carbonate solution
6. extractionthe mixture was extracted with chloroform
7. washThe organic layer was washed with a saturated brine
8. dry with materialdried over sodium sulfate
9. customthe solvent was evaporated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (chloroform: methanol (50:1))
11. customcrystallized from isopropyl alcohol