反应详情

To a solution of 4-amino-1-methanesulfonyl-1H-pyrrole-2-carboxylic acid ethyl ester (1 g, 4.3 mmol) and triethylamine (650 mg, 6.4 mmol) in dry CH2Cl2 (20 mL) was added 2,3-difluoro-benzoyl chloride (760 mg, 4.3 mmol). The mixture was stirred at RT for 3 h and diluted with EtOAc (150 mL). After washing with 2N HCl (80 mL) and NaHCO3 (2×80 mL), the organic layer was dried over MgSO4, filtered, and evaporated to give a yellow solid (1.3 g, 81%). This solid was dried on the vacuum pump for 14 hrs and then was used for the next step directly. MS (ES+): m/e=373.2 (M+H); LC: 3.45 min.

1. washAfter washing with 2N HCl (80 mL) and NaHCO3 (2×80 mL)
2. dry with materialthe organic layer was dried over MgSO4
3. filtrationfiltered
4. customevaporated