反应详情

温度

100 °C

A mixture of 2-[(3-chloro-2-fluoro-phenylamino)-(4-chloro-2-methyl-phenyl)-methyl]-1-isopropyl-1H-pyrrole-3-carboxylic acid ethyl ester (Step A3) (2.154 mmol) and 1N aqueous LiOH (8.62 mmol) in dioxane (25 mL) was heated at 100° C. for 26 h. After cooling to rt, the reaction mixture was partitioned between EtOAc and 10% w/w aqueous citric acid. The aqueous phase was extracted with EtOAc (2×). The combined organic phases were dried (Na2SO4), filtered and concentrated to afford the title compound as a pale yellow solid which was used in the next step without further purification. tR: 5.48 min (HPLC 1); ESI-MS: tR=1.33 min, [M−H] 433/435 (LC-MS 1).

1. temperatureAfter cooling to rt
2. customthe reaction mixture was partitioned between EtOAc and 10% w/w aqueous citric acid
3. extractionThe aqueous phase was extracted with EtOAc (2×)
4. dry with materialThe combined organic phases were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated