反应详情

To a stirred solution of ethyl 4-(quinoline-8-sulfonamido)benzoate 90 (8 gm, 22.4 mmol) in THF:H2O (1:1) under nitrogen atmosphere was added solid LiOH (9.4 gm, 224 mmol) at RT. The solution was then refluxed for 6 hr. After completion of the reaction, the reaction mixture was washed with ethyl acetate (2×100 ml) to remove non polar impurities. The aqueous layer was acidified (pH 4) with citric acid solution. The resultant precipitate was filtered out and air-dried. The traces of water were removed by co-distillation with toluene. The resultant off white solid (5.9 gm, 80%) was taken to the next step without further purification.

1. temperatureThe solution was then refluxed for 6 hr
2. customAfter completion of the reaction
3. washthe reaction mixture was washed with ethyl acetate (2×100 ml)
4. customto remove non polar impurities
5. filtrationThe resultant precipitate was filtered out and
6. customair-dried
7. customThe traces of water were removed by co-distillation with toluene
8. customThe resultant off white solid (5.9 gm, 80%) was taken to the next step without further purification