反应详情

To 2-Fluoro-5-(propane-1-sulfonylamino)-benzoic acid methyl ester (670, 1.20 g, 0.00436 mol) in tetrahydrofuran (100.0 mL) was added lithium tetrahydroaluminate (1.00 M in tetrahydrofuran, 10.0 mL) under an atmosphere of nitrogen. The reaction was stirred at room temperature overnight. To the reaction was added Na2SO4.10H2O (5 g), and then stirred at room temperature for 1 hour. The reaction was filtered, concentrated and purified with silica gel column chromatography eluting with 50% ethyl acetate in hexane to give the compound (671, 0.90 g, 83%). MS (ESI) [M−H+]−=246.1.

1. stirringstirred at room temperature for 1 hour
2. filtrationThe reaction was filtered
3. concentrationconcentrated
4. custompurified with silica gel column chromatography
5. washeluting with 50% ethyl acetate in hexane
6. customto give the compound (671, 0.90 g, 83%)