Sulfuryl chloride → HCID 13749915, compound

Participants

Reaction Steps

The chloroform solution of ethyl 2-carboethoxy-3,4-dimethoxybenzenecarbamate prepared in A above was treated with sulfuryl chloride (30.2 g, 0.22 mole) and optionally with sodium bicarbonate (33.3 g, 0.40 mole) and the mixture was stirred at room temperature for 4 hours. An additional charge of sodium bicarbonate (3.3 g, 0.04 mole) and sulfuryl chloride (3.0 g, 0.02 mole) was added and stirring was continued for 16 hours. Filtration and concentration of the filtrate provided crude product as an oil which was crystallized from aqueous methanol. The resultant solid was dissolved in chloroform and the solution was dried, filtered and concentrated to give an oil which was crystallized from hexanes; 37.3 g (85%), mp 111°-113° C.

Provenance & Evidence