反应详情

温度

40 °C

A mixture of 6-(2-Amino-5-bromo-phenylcarbamoyl)-5-aza-spiro[2.4]heptane-5-carboxylic acid benzyl ester and 6-(2-Amino-4-bromo-phenylcarbamoyl)-5-aza-spiro[2.4]heptane-5-carboxylic acid benzyl ester (1.446 g, 3.25 mmol) was dissolved in AcOH (20 mL) and the reaction mixture was stirred at 40° C. for 18 hours then concentrated under reduced pressure. The residue was dissolved in EtOAc and washed with saturated aqueous NaHCO3. The aqueous layer was extracted 2× with EtOAc and the combined organics were dried over MgSO4, filtered and concentrated to provide 6-(6-Bromo-1H-benzoimidazol-2-yl)-5-aza-spiro[2.4]heptane-5-carboxylic acid benzyl ester (1.385 g, 100%).

1. concentrationthen concentrated under reduced pressure
2. dissolutionThe residue was dissolved in EtOAc
3. washwashed with saturated aqueous NaHCO3
4. extractionThe aqueous layer was extracted 2× with EtOAc
5. dry with materialthe combined organics were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated