Ammonium Chloride → HCID 11276762, compound

Participants

Reaction Conditions

Reaction Steps

67.9 g (0.27 mol) of methyl 3-(3-methyl-2-butenylthio)-2-methylbenzoate were dissolved in 600 ml of methylene chloride and, at −5 to 0° C., 206.4 g (1.09 mol) of titanium tetrachloride in 600 ml of methylene chloride were added dropwise, and the mixture was stirred at 0° C. for three hours. The mixture was subsequently stirred into 1.5 kg of ice and 500 ml of saturated ammonium chloride solution, the organic phase was separated off and dried and the solvent was removed. This gave 62.9 g of an orange oil which was directly used further. To characterize the product, a sample was chromatographed over silica gel (mobile phase: cyclohexane/ethyl acetate=10/1).

Provenance & Evidence