反应详情

Into a 250 milliliter reaction flask equipped with a magnetic stirrer was added 10.04 grams (0.044 moles) of 3,4,5-trichloronitrobenzene, 8.16 grams (0.044 moles) of 2-phenylbenzyl alcohol, 1.29 grams (0.004 moles) of tetra-N-butylammonium bromide, 80 milliliters of toluene and aqueous sodium hydroxide (5.28 grams in 6.6 milliliters of water). The resulting mixture was stirred vigorously at ambient temperature overnight. The mixture was then diluted with water and filtered. The layers were separated and the organic layer was washed twice with water and finally once with a saturated aqueous sodium chloride solution. After drying over anhydrous sodium sulfate, the mixture was concentrated under vacuum to give a red-orange oil which was stirred into hexane. Crystallization from the hexane and filtration afforded a yellow-orange powder having a melting point of 83.0° C.-84.5° C.

1. customInto a 250 milliliter reaction flask
2. customequipped with a magnetic stirrer
3. filtrationfiltered
4. customThe layers were separated
5. washthe organic layer was washed twice with water and finally once with a saturated aqueous sodium chloride solution
6. dry with materialAfter drying over anhydrous sodium sulfate
7. concentrationthe mixture was concentrated under vacuum
8. customto give a red-orange oil which
9. customCrystallization
10. filtrationfrom the hexane and filtration
11. customafforded a yellow-orange powder