反应详情

To a solution of 5.0 g (0.014 mole) of 4,5-diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole in 50 ml of THF was added dropwise 15 ml of 1.6 M methyl lithium solution, followed by a solution of 5.5 g (0.045 mole) of dimethylthiocarbamoyl chloride in 25 ml THF. The reaction mixture was heated at reflux several hours, then concentrated by rotary evaporation. The residue was shaken with ether and 1 N hydrochloric acid. The ether layer was washed with 10% sodium bicarbonate solution, then dried and concentrated. The residue (7.8 g) was purified by chromatography on silica gel, eluting with toluene to give 0.8 g of product, mp 133°-133.5° (recrystallized from methyl cyclohexane).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux several hours
3. concentrationconcentrated by rotary evaporation
4. washThe ether layer was washed with 10% sodium bicarbonate solution
5. customdried
6. concentrationconcentrated
7. customThe residue (7.8 g) was purified by chromatography on silica gel
8. washeluting with toluene
9. customto give
10. custom0.8 g of product, mp 133°-133.5° (recrystallized from methyl cyclohexane)