反应详情

To a solution of benzyloxycarbonylamino-hydroxy-acetic acid (5.9 g, 26.2 mmol) (prepared according to the procedure of E. H. W. Bohme, et al., J. Med. Chem, 1980, 23, 405-412) and 2-methylanisole (3.2 g, 26.2 mmol) in acetic acid (150 mL) was added concentrated sulfuric acid (15 mL). The mixture was stirred at room temperature for 1 hour, then poured into ice/water and extracted with ethyl acetate (2×200 mL). The combined organic extracts were dried over sodium sulfate and concentrated to give an oily residue. The residue was triturated in hexanes, the precipitate formed was collected by filtration and dried overnight to give crude benzyloxycarbonylamino-(4-methoxy-3-methyl-phenyl)-acetic acid as a white solid (8.6 g, 100%).

1. extractionextracted with ethyl acetate (2×200 mL)
2. dry with materialThe combined organic extracts were dried over sodium sulfate
3. concentrationconcentrated
4. customto give an oily residue
5. customThe residue was triturated in hexanes
6. customthe precipitate formed
7. filtrationwas collected by filtration
8. customdried overnight