Sulfuryl chloride → HCID 12832645, compound

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.

1. stirringThe mixture is stirred for about 7 hours at 50°
2. customThe mixture is then quenched
3. additionby pouring into water
4. extractionThe resulting mixture is then extracted with methylene chloride
5. washThe combined extracts are washed with 10% aq. sodium bicarbonate solution
6. dry with materialbrine, dried over anh. sodium sulfate
7. concentrationconcentrated (under vacuum)
8. customto obtain an oily residue
9. distillationThe oil is distilled under vacuum (0.01 mm Hg) at 100° (constant boiling point)
10. customto obtain an oil which
11. distillationis re-distilled (at 0.001 mm Hg) at 90° C. for 1/2 hr

ORD record

ord-73a3ee1f178149ad864652c1129d94f0

Source dataset

uspto-grants-1982_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04321269