Sulfuryl chloride → HCID 12832645, compound

Participants

Reaction Steps

To a hot (50°) solution of the product of step B in 20 ml chloroform, 2.61 g (1.55 ml) of sulfuryl chloride is added dropwise (using a syringe) with vigorous stirring over a period of from 10 to 15 minutes. The mixture is stirred for about 7 hours at 50°. The mixture is then quenched by pouring into water. The resulting mixture is then extracted with methylene chloride. The combined extracts are washed with 10% aq. sodium bicarbonate solution then brine, dried over anh. sodium sulfate, then concentrated (under vacuum) to obtain an oily residue. The oil is distilled under vacuum (0.01 mm Hg) at 100° (constant boiling point) to obtain an oil which is re-distilled (at 0.001 mm Hg) at 90° C. for 1/2 hr. to obtain refined title product.

Provenance & Evidence