反应详情

温度

110 °C

To a mixture of 5-chloro-2-(3-(4-(trifluoromethyl)phenoxy)azetidin-1-yl)nicotinic acid (D104) (200 mg, 0.53 mmol), methyl 4-(1-aminocyclopropyl)benzoate (D7) (144.31 mg, 0.634 mmol) and N,N-diisopropylethylamine (0.291 ml, 1.674 mmol) in dichloromethane (8 ml), ®T3P (1-Propanephosphonic acid cyclic anhydride) (403 mg, 0.633 mmol) was added and the mixture stirred under microwave irradiation at 110° C. for 10 min (2 cycle of 5 min each). 1M NaOH (5 ml) was added and the mixture extracted with dichloromethane (3×20 ml). Collected organics, after solvent evaporation, afforded a crude material that was purified by SPE-Si cartridge (10 g) eluting with a mixture cyclohexane/ethyl acetate from 100/0 to 60/40. Collected fractions, after solvent evaporation, afforded the title compound (D148) (140 mg)

1. additionwas added
2. extractionthe mixture extracted with dichloromethane (3×20 ml)
3. customCollected organics, after solvent evaporation
4. customafforded a crude material that
5. customwas purified by SPE-Si cartridge (10 g)
6. washeluting with a mixture cyclohexane/ethyl acetate from 100/0 to 60/40
7. customCollected fractions, after solvent evaporation