反应详情

温度

0 °C

To 40 mg (0.14 mmol) of 5-bromo-4-methoxy-3-methyl-benzofuran-2-carboxylic acid was added 0.5 mL of oxalyl chloride and the mixture was refluxed for 2 h, then the excess oxalyl chloride was removed by vacuum. The residue was dissolved in 0.5 mL of dichloromethane and was added to a mixture of 92 mg (0.25 mmol) of (S)-2-(4′-amino-biphenyl-4-sulfonylamino)-3-methyl-butyric acid methyl ester, 34 mg (0.28 mmol) of 4-(dimethylamino)pyridine and 1 mL of dichloromethane in an ice/water bath. The mixture was stirred at 0° C. for overnight. The mixture was diluted with dichloromethane and was washed with 2N HCl, and water. Removal of the solvent from the organic solution gave 20 mg (23% yield) of (S)-2-{4′-[(5-bromo-4-methoxy-3-methyl-benzofuran-2-carbonyl)-amino]-biphenyl-4-sulfonylamino}-3-methyl-butyric acid methyl ester as an off-white solid.

1. temperaturethe mixture was refluxed for 2 h
2. customthe excess oxalyl chloride was removed by vacuum
3. dissolutionThe residue was dissolved in 0.5 mL of dichloromethane
4. washwas washed with 2N HCl, and water
5. customRemoval of the solvent from the organic solution