反应详情

A solution of acid 4 (160 mg), EDCI (90 mg), and N-hydroxysucinimide (53 mg) in DMF (2 mL) was reacted at rt overnight. Water (12 ml) was added and the solution was extracted with EtOAc (15 mL×2), dried over Na2SO4. Evaporation of solvent gave a residue, into which EtOAc (4 mL) and 2-propylamine (1.2 eq) was added. The reaction was kept at rt for 1 h., then concentrated and the crude product purified by column chromatography to give the desired product (yield: 80%). HPLC (4 minute gradient) tR=2.00 min; MS m/z 446.19 [M+H]+.

1. extractionthe solution was extracted with EtOAc (15 mL×2)
2. dry with materialdried over Na2SO4
3. customEvaporation of solvent
4. customgave a residue
5. concentrationconcentrated
6. customthe crude product purified by column chromatography