反应详情

A mixture of 1-(3-chlorophenyl)-3-methylcyclohexan-1-ol (25.0 g, 0.11 mole) and sulfur (7.1 g, 0.22 mole) was heated at 250° for 4.5 hours. The reaction mixture then stood at room temperature for approximately 60 hours, and then it was distilled under reduced pressure to give 19.5 grams of distillate; bp, 150°-165°/10 mm. The distillate was chromatographed on silica gel, elution with hexane. The eluent was evaporated under reduced pressure to give 3'-chloro-3-methyl[1,1'-biphenyl] (17.0 g) as an oil. The nmr and the ir spectra of the oil were consistent with the proposed structure.

1. temperaturewas heated at 250° for 4.5 hours
2. distillationit was distilled under reduced pressure
3. customto give 19.5 grams of distillate
4. custombp, 150°-165°/10 mm
5. distillationThe distillate was chromatographed on silica gel, elution with hexane
6. customThe eluent was evaporated under reduced pressure