反应详情

A solution of L-t-leucine methyl ester (1.00 g, 6.89 mmol), 6-heptenoic acid (1.06 g, 8.26 mmol), EDC (1.58 g, 8.26 mmol) and HOAt (1.23 g, 8.26 mmol) in DMF (10 mL) was stirred at 22° C. for 2 hours. The reaction mixture was diluted with aqueous saturated NaHCO3 (30 mL), and extracted with EtOAc (3×50 mL). The combined organic layers were washed with water (3×30 mL), brine (20 mL), dried over Na2SO4, filtered and concentrated. The residue was chromatographed on silica gel, eluting with 5-50% EtOAc/hexane, to give the title product (1.42 g, 81%). LRMS (ESI) m/z 256.3 [(M+H)+; calcd for C14H26NO3: 256.2].

1. extractionextracted with EtOAc (3×50 mL)
2. washThe combined organic layers were washed with water (3×30 mL), brine (20 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was chromatographed on silica gel
7. washeluting with 5-50% EtOAc/hexane