反应详情

DPP-Cl (43 μl) and TEA (31 μl) were added to a solution of 3-acetoxy-2-methylbenzoic acid (41 mg) in EtOAc (2 ml), and the mixture was stirred for one hour. After the addition of the compound obtained in Step 2 (85 mg) and TEA (34 μl), the mixture was stirred overnight. The reaction mixture was washed with 5% Na2CO3 (×2), 1N HCl, and 5% NaCl. After concentration, MeOH (1.5 ml) and 1N NaOH (300 μl) were added. After stirring for one hour, IN HCl was added to make the reaction mixture acidic. The resulting mixture was extracted with EtOAc. The extract was washed with 5% Na2CO3 (×2), 1N HCl, and 5% NaCl, dried over MgSO4, filtered and concentrated. The residue was recrystallized from a mixture of EtOAc and n-hexane to obtain the title compound (90 mg, 81%).

1. stirringthe mixture was stirred overnight
2. washThe reaction mixture was washed with 5% Na2CO3 (×2), 1N HCl, and 5% NaCl
3. concentrationAfter concentration, MeOH (1.5 ml) and 1N NaOH (300 μl)
4. additionwere added
5. stirringAfter stirring for one hour, IN HCl
6. additionwas added
7. extractionThe resulting mixture was extracted with EtOAc
8. washThe extract was washed with 5% Na2CO3 (×2), 1N HCl, and 5% NaCl
9. dry with materialdried over MgSO4
10. filtrationfiltered
11. concentrationconcentrated
12. customThe residue was recrystallized from a mixture of EtOAc and n-hexane