反应详情

To a solution of benzo[b]thiophene-2-sulfonic acid [2-(2-chloro-5-trifluoromethylbenzenesulfonylamino)phenyl]-amide (0.5 mmol) in dioxane (5 mL), solid sodium methoxide (2 mmol) was added in one portion and the resulting reaction mixture was then heated to reflux for ca. 4 h. After the completion of the reaction, the reaction mixture was cooled to RT and concentrated in vacuo. The residue obtained was redissolved in EtOAc (10 mL) and was washed with water (10 mL) and brine (10 mL). The organic phase was dried over anhydrous sodium sulfate and concentrated under vacuum. The residue obtained was purified by flash column chromatography eluting with DCM/EtOAc to obtain 204 mg of benzo[b]thiophene-2-sulfonic acid [2-(2-methoxy-5-trifluoromethyl-benzenesulfonylamino)phenyl]-amide. LC: Tr 1.20 min; MS: 544.1 (M+1)+.

1. customthe resulting reaction mixture
2. temperaturewas then heated
3. temperatureto reflux for ca. 4 h
4. customAfter the completion of the reaction
5. concentrationconcentrated in vacuo
6. customThe residue obtained
7. washwas washed with water (10 mL) and brine (10 mL)
8. dry with materialThe organic phase was dried over anhydrous sodium sulfate
9. concentrationconcentrated under vacuum
10. customThe residue obtained
11. customwas purified by flash column chromatography
12. washeluting with DCM/EtOAc