Hydrochloric Acid → HCID 14972913, compound

Participants

Reaction Steps

Into 30 ml of dried pyridine, was dissolved 1.78 g of 1-(1-hydroxy-1-methylethyl)benzocyclobutene. To the solution, was added dropwise 3.37 g of phosphorus oxychloride over a period of 5 minutes at room temperature. The mixture was stirred for 24 hours at room temperature, then poured into 3% aqueous cold hydrochloric acid solution and admixed with ether. After the ether layer was separated, the aqueous layer was extracted twice with ether. The ether layers were combined, washed with saturated aqueous sodium hydrogencarbonate solution, then with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain as the residue 1.5 g of a mixture of the intended product and 1-isopropenylbenzocyclobutene. This mixture was used without further purification as the starting material in the next step of preparation.

Provenance & Evidence