反应详情

To 7.2 mmol 5-cyclopropanesulfonyl-2-hydroxy-benzoic acid in 20 ml dichloroethane containing a few drops of DMF was added dropwise 8.7 mmol oxalyl chloride. After stirring for 90 min at RT, the reaction mixture was cooled to 0° C. and then 144 mmol methanol was added, followed by 72 mmol pyridine, and stirring continued at RT for 1 h. The mixture was then washed with 1 M aq HCl, dried with Na2SO4, and concentrated in vacuo. The residue was chromatographed on silica gel (eluant: ethyl acetate/heptane gradient) to afford the title compound. MS (m/e): 255.2 ([M−H]−, 100%)

1. temperaturethe reaction mixture was cooled to 0° C.
2. stirringstirring
3. waitcontinued at RT for 1 h
4. washThe mixture was then washed with 1 M aq HCl
5. dry with materialdried with Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was chromatographed on silica gel (eluant: ethyl acetate/heptane gradient)