反应详情

温度

80 °C

A mixture of 2-[(3-chloro-2-fluoro-phenylamino)-(4-chloro-2-methyl-phenyl)-methyl]-1-isopropyl-1H-pyrrole-3-carboxylic acid (Step A2) (2.257 mmol), HATU (2.482 mmol) and NMM (6.77 mmol) in DMF (30 mL) was heated at 80° C. for 18 h. After cooling to rt, the reaction mixture was diluted with EtOAc and washed with a saturated aqueous solution of NaHCO3. The aqueous phase was extracted with EtOAc (2×). The combined organic phases were washed with brine, dried (Na2SO4), filtered and concentrated. The residue was purified using a RediSep® silica gel column to afford the title compound as a white solid. tR: 5.31 min (HPLC 1); ESI-MS: tR=1.29 min, [M+H]+ 417/419 (LC-MS 1); TLC: Rf=0.13 (1:3 EtOAc/heptanes).

1. temperatureAfter cooling to rt
2. washwashed with a saturated aqueous solution of NaHCO3
3. extractionThe aqueous phase was extracted with EtOAc (2×)
4. washThe combined organic phases were washed with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified