反应详情

3-[(N-Benzyl-N-cyclopropanecarbonyl-amino)-methyl]-4-bromo-benzoic acid (0.1 g, 0.26 mmol) and catalytic DMF (0.01 mL) were combined in CH2Cl2 (4 mL) at room temperature. Oxalyl chloride (0.03 mL, 0.33 mmol) was added, and the reaction was stirred for 30 minutes. The solution was concentrated and dried under vacuum, and then NMP (3 mL) and diisopropylethylamine (0.14 mL, 0.78 mmol) were added. Benzylamine (0.04 mL, 0.39 mmol) was then added, and the reaction was stirred for 5 minutes. The mixture was poured into H2O and partitioned with 1:1 EtOAc:hexanes. The organic layer was washed with saturated aqueous NaHCO3, H2O, and dilute brine, and then dried, filtered, and concentrated to give N-benzyl-3-[(N-benzyl-N-cyclopropanecarbonyl-amino)-methyl]-4-bromo-benzamide.

1. concentrationThe solution was concentrated
2. customdried under vacuum
3. stirringthe reaction was stirred for 5 minutes
4. custompartitioned with 1:1 EtOAc
5. washThe organic layer was washed with saturated aqueous NaHCO3, H2O, and dilute brine
6. customdried
7. filtrationfiltered
8. concentrationconcentrated