反应详情

A mixture of 3.5 g (0.01 mole) of 4,5-diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole, 2.1 g (0.013 mole) benzyl chloromethyl ether, 3.6 g (0.026 mole) potassium carbonate in 25 ml DMF was stirred for 24 hours. TLC showed some starting material, so an additional 0.5 g (0.003 mole) of benzyl chloromethyl ether was added and stirring continued for another 24 hours. The mixture was poured into ice water, extracted three times with ether and the ether layers backwashed three times with water. The ether solution was dried and concentrated on a rotary evaporator. The residue was chromatographed on 200 g SilicAR CC-7, eluting with toluene to give, after recrystallization from hexane, 3.6 g (76.6%) of white product, mp 70°-70.5°.

1. stirringstirring
2. waitcontinued for another 24 hours
3. extractionextracted three times with ether
4. dry with materialThe ether solution was dried
5. concentrationconcentrated on a rotary evaporator
6. customThe residue was chromatographed on 200 g SilicAR CC-7
7. washeluting with toluene
8. customto give
9. customafter recrystallization from hexane, 3.6 g (76.6%) of white product, mp 70°-70.5°