反应详情

(5-Trifluoromethyl-benzo[d]isoxazol-3-ylamino)-acetic acid (2.6 g, 9.99 mmol), 3-amino-azetidine-1-carboxylic acid tert-butyl ester (1.72 g, 9.99 mmol), EDCI (2.3 g, 12.0 mmol), HOBt (1.62 g, 12.0 mmol) in DCM (20 mL) were stirred at room temperature for 4 hours. The reaction was then partitioned between DCM and water. The aqueous layer was extracted two times with DCM. The combined organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give the crude material, which was purified by silica gel column (hexanes:ethyl acetate 1:1) to afford the title compound as white foam.

1. customThe reaction was then partitioned between DCM and water
2. extractionThe aqueous layer was extracted two times with DCM
3. washThe combined organic layer was washed with brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customto give the crude material, which
8. customwas purified by silica gel column (hexanes:ethyl acetate 1:1)