反应详情

To a suspension of N-{[2-(Aminocarbonyl)-5-chloro-1H-indol-3-yl]sulfonyl}-N-methylglycine from Example 56 (10 mg, 0.029 mmol) in 1 mL of dichloromethane at room temperature was added oxalyl chloride (0.3 mL), followed by DMF (ca. 0.020 mL). After 20 minutes, the homogeneous mixture was concentrated in vacuo to give a yellow solid. This was taken up in 1 mL of acetone, and a solution of 10% NH4OH/acetone (2 mL) was added, whereupon a white precipitate formed. After two minutes, the solvent was decanted off, and the resulting solid was maintained in vac o until dry. Purification by preparative reversed phase HPLC provided the titled compound as a white solid. ESI+ MS: 345.2 [M+H]+.

1. concentrationthe homogeneous mixture was concentrated in vacuo
2. customto give a yellow solid
3. customformed
4. waitAfter two minutes
5. customthe solvent was decanted off
6. temperaturethe resulting solid was maintained in vac o
7. customuntil dry
8. customPurification by preparative reversed phase HPLC