Hydrochloric Acid → HCID 70373902, compound

Under a dry nitrogen atmosphere, 7.18 g (0.0914 mole) of acetyl chloride was added to a cold (5° C.), stirred mixture of 11.9 g (0.0893 mole) of aluminum chloride in 100 ml of carbon tetrachloride. To this mixture was added a solution of 10.6 g (0.079 mole) of thianaphthalene in 25 ml of carbon tetrachloride. The reaction mixture was allowed to warm to room temperature and was stirred for two hours. The mixture was heated at reflux for 45 minutes and was cooled. The resultant mixture was poured into ice water, and 100 ml of concentrated hydrochloric acid was added. This mixture was stirred until the ice melted. The organic phase was removed and saved. The aqueous phase was extracted with methylene chloride. The organic phases were combined and dried over anhydrous sodium sulfate. This mixture was filtered, and the filtrate was treated with silica gel and decolorizing charcoal. The resulting mixture was filtered through a pad of silica gel. The filtrate was evaporated under reduced pressure to yield 11.3 g of 2 -acetylthianaphthalene as an oil.

1. stirringwas stirred for two hours
2. temperatureThe mixture was heated
3. temperatureat reflux for 45 minutes
4. temperaturewas cooled
5. additionwas added
6. customThe organic phase was removed
7. extractionThe aqueous phase was extracted with methylene chloride
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationThis mixture was filtered
10. additionthe filtrate was treated with silica gel
11. filtrationThe resulting mixture was filtered through a pad of silica gel
12. customThe filtrate was evaporated under reduced pressure

ORD record

ord-f54050c5a9664a059881e83d6a8d612b

Source dataset

uspto-grants-1990_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04908357