反应详情

Chlorosulfonic acid (5.8 g, 49 mmol) was cooled to 0° C., then 2,2,2-trifluoro-N-(3-(2-(methylsulfonyl)ethyl)phenyl)acetamide (2 g, 6.8 mmol) was added slowly. The reaction mixture was allowed to warm to room temperature. Two hours later, the reaction was poured onto ice. The aqueous layer was extracted with ethyl acetate 3 times. The combined organic phase was washed with brine, dried over sodium sulfate. The crude product was purified by pre-HPLC (column: Luna 300×50.0 mm, 10 um; liquid phase: [A-H2O+0.05% TFA; B-MeCN] B %: 0%-27%, 23 min) to give 2-(2-(methylsulfonyl)ethyl)-4-(2,2,2-trifluoroacetamido)benzenesulfonic acid (1.1 g, yield 28%).

1. additionTwo hours later, the reaction was poured onto ice
2. extractionThe aqueous layer was extracted with ethyl acetate 3 times
3. washThe combined organic phase was washed with brine
4. dry with materialdried over sodium sulfate
5. customThe crude product was purified by pre-HPLC (column: Luna 300×50.0 mm, 10 um; liquid phase: [A-H2O+0.05% TFA; B-MeCN] B %: 0%-27%, 23 min)