反应详情

温度

70 °C

206 mg (1.5 mmol) K2CO3 and 303 mg (1.5 mmol) 2-(phenylsulfonyl)ethanethiol were added to a solution of 827 mg (1.0 mmol) 2-chloro-6-(trifluoromethyl)quinoline-3-carboxylic acid (precursor VVV03) in acetone (3 ml) and the mixture was heated for 5 h at 70° C. Then it was filtered and the filtrate was concentrated to small volume under vacuum. The residue was dissolved in water and acidified with a 1N hydrochloric acid. It was then extracted with EE and the organic phase was dried over Na2SO4, filtered and concentrated to small volume under vacuum. Crystallisation (DCM/hexane) of the residue yielded 316 mg (0.7 mmol, 72%) 2-(2-(phenylsulfonyl)ethylthio)-6-(trifluoromethyl)quinoline-3-carboxylic acid.

1. filtrationThen it was filtered
2. concentrationthe filtrate was concentrated to small volume under vacuum
3. dissolutionThe residue was dissolved in water
4. extractionIt was then extracted with EE
5. dry with materialthe organic phase was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated to small volume under vacuum
8. customCrystallisation (DCM/hexane) of the residue