反应详情

温度

-5 °C

was prepared using a literature procedure (Asprou et al., J. Heterocyclic Chem., 17:87-92 (1980) (“Asprou”), which is hereby incorporated by reference). To a 50 mL round bottom flask charged with a stir bar was added 4-keto-4,5,6,7-tetrahydrothianaphthene (0.61 g, 4 mmole) and concentrated sulfuric acid (6 mL). The solution was then cooled in an ice/salt bath to −5° C. and stirred while a solution of concentrated nitric acid (0.3 mL) in concentrated sulfuric acid (3 mL) was added dropwise over 30 minutes. Solution was stirred for another 50 minutes and allowed to gradually warm to 5° C. The reaction mixture was then poured onto crushed ice and the yellow precipitate filter and washed with several portions of ice-cold water to give product as a yellow solid (0.594 g, 75% yield). Spectral data were consistent with the literature values (Asprou, which is hereby incorporated by reference).

1. customwas prepared
2. additionTo a 50 mL round bottom flask charged with a stir bar
3. additionwas added dropwise over 30 minutes
4. temperatureto gradually warm to 5° C
5. additionThe reaction mixture was then poured
6. customonto crushed ice
7. filtrationthe yellow precipitate filter
8. washwashed with several portions of ice-cold water