反应详情

[step 1] 3,3-Difluorocyclobutanecarboxylic acid (500 mg, 3.67 mmol) was dissolved in DMF (18 mL), 1,1′-carbonyldiimidazole (1.19 g, 7.35 mmol) was added, and the mixture was stirred at room temperature for 1 hr. To the mixture were added 2-nitroaniline (1.02 g, 7.35 mmol) and triethylamine (1.02 mL, 7.35 mmol), and the mixture was stirred at 80° C. for 13 hr. To the mixture were added 5% aqueous citric acid solution and ethanol (5 mL), and the mixture was stirred for 1 hr. The precipitated crystals were collected by suction filtration to give 3,3-difluoro-N-(2-nitrophenyl)cyclobutanecarboxamide (527 mg, 56%).

1. stirringthe mixture was stirred at 80° C. for 13 hr
2. stirringthe mixture was stirred for 1 hr
3. filtrationThe precipitated crystals were collected by suction filtration