反应详情

To a suspension of 5-[4-fluoro-2-(trifluoromethyl)phenyl]-4-methyl-1H-pyrrole-3-carboxylic acid (7.7 g, 27 mmol) in dichloromethane (60 ml) was added oxalyl chloride (5.1 ml, 59 mmol). The mixture was stirred at room temperature for 2.0 h, after which time the solvent was removed on a rotary evaporator. To this brown residue was added 4-(methanesulfonyl)aniline hydrochloride (5.8 g, 28 mmol), tetrahydrofuran (THF) (80 ml) and diisopropylethylamine (DIEA) (14 ml, 80 mmol). The solution was stirred at room temperature for 2.0 h. The reaction mixture was concentrated and to the residue was added 2N HCl (80 ml) and water (80 ml) and resulting suspension was stirred for 30 min. The solid was filtered and washed with water and diisopropyl ether (IPE) to give the title compound as a white solid (11 g, 90%).

1. customafter which time the solvent was removed on a rotary evaporator
2. stirringThe solution was stirred at room temperature for 2.0 h
3. concentrationThe reaction mixture was concentrated and to the residue
4. additionwas added 2N HCl (80 ml) and water (80 ml)
5. customresulting suspension
6. stirringwas stirred for 30 min
7. filtrationThe solid was filtered
8. washwashed with water and diisopropyl ether (IPE)