p-Toluenesulfonic acid → HCID 20432292, compound

Participants

Reaction Steps

319 g (1 mol) of 8-bromo-10,11-dimethyl-dihydrodibenz[b,f]oxepin-10-ol (crude product) and 1.5 g of p-toluenesulfonic acid are heated in a distillation apparatus under 11 mm Hg for 1 hour at an external temperature of 180° and for 5 hours at an external temperature of 200°, water being eliminated. The distillation receiver is then changed and the 2-bromo-10,11-dimethyldibenz[b,f]oxepine formed is then distilled under a high vacuum; boiling point 142°-148°/0.01 mm Hg. The pale yellow distillate is dissolved in 300 ml of acetonitrile and the solution is cooled to 0°, whereupon the product crystallises out; melting point 117°-119°.

Provenance & Evidence