反应详情

温度

0 °C

336 mg (3.0 mmol) potassium tert-butylate were added to a solution of 360 mg (3.0 mmol) 3-mercaptopropionic acid methyl ester in DMF (8 ml) at 0° C. and the mixture was stirred for 30 min at 0° C. Then 953 mg (3.0 mmol) 2-chloro-4-methyl-7-(trifluoromethyl)quinoline-3-carboxylic acid ethyl ester were added and the reaction solution was heated slowly to 50° C. and stirred for 16 h at this temperature. After cooling to RT the mixture was diluted with water and extracted with EE. The organic phase was dried over MgSO4, filtered and concentrated to small volume under vacuum. Column chromatography (hexane/EE 9:1) of the residue yielded 625 mg (1.5 mmol, 50%) 2-(3-ethoxy-3-oxopropylthio)-4-methyl-7-(trifluoromethyl)quinoline-3-carboxylic acid ethyl ester.

1. temperaturethe reaction solution was heated slowly to 50° C.
2. stirringstirred for 16 h at this temperature
3. temperatureAfter cooling to RT the mixture
4. extractionextracted with EE
5. dry with materialThe organic phase was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated to small volume under vacuum