反应详情

A solution of 2-(3-amino-4-hydroxy-phenyl)-propionic acid ethyl ester (370 mg) in DMF (2 mL) was added phenyl chlorothionoformate (380 mg in DMF), and DBU (540 mg, in DMF) at room temperature. The reaction mixture was stirred for 16 h at room temperature and water was added to this mixture. The resulting mixture was extracted with ethyl ether. The combined organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The resulting residue was chromatographed on silica gel (n-Hex:EtOAc=4:1) to afford the product as white solid. (130 mg, 29.2%)

1. extractionThe resulting mixture was extracted with ethyl ether
2. dry with materialThe combined organic layer was dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe resulting residue was chromatographed on silica gel (n-Hex:EtOAc=4:1)