Thiirane → HCID 23035065, compound

A solution of silver nitrate (1.84 g, 10.6 mmol) in water (5 ml) was added to a stirred aqueous solution (20 ml) of 4-pyridine ethane sulfonic acid (2.00 g, 10.6 mmol) which had been adjusted to pH 7 by the addition of aqueous 2.5N sodium hydroxide (3.0 ml). The solution was cooled in an ice-water bath and ethylene sulfide (0.71 ml, 11.8 mmol) added. The resulting mixture was let stand 45 minutes at ice-bath temperature and the upper clear phase decanted. The gummy solid was mixed with water (20 ml) and vigorously bubbled with hydrogen sulfide for 15 minutes. After stirring an additional 20 minutes, the mixture was filtered through a celite pad to remove silver sulfide and the filtrate was evaporated under vacuum to provide crude title compound as a white semi-solid (1.00 g).

1. temperatureThe solution was cooled in an ice-water bath
2. customtemperature and the upper clear phase decanted
3. additionThe gummy solid was mixed with water (20 ml)
4. customvigorously bubbled with hydrogen sulfide for 15 minutes
5. filtrationthe mixture was filtered through a celite pad
6. customto remove silver sulfide
7. customthe filtrate was evaporated under vacuum

ORD record

ord-5b0d0b9100594a73b71f0bd0bd024eba

Source dataset

uspto-grants-1990_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04952397