反应详情

温度

0 °C

1M Lithium hydroxide (57 μl) is added dropwise to a cooled (0° C.) solution of [1-(4-cyano-3-ethoxy-benzenesulfonyl)-2-methyl-1H-pyrrolo[2,3-b]pyridin-3-yl]-acetic acid methyl ester (0.024 g, 0.057 mmol) in THF/water (4 ml of a 1:1 mixture). After stirring at 0° C. for 10 minutes, the reaction mixture is stirred at room temperature for 2.5 hours and then diluted with DCM (4 ml). The resulting mixture is passed through a phase separation cartridge and the aqueous portion is acidified to pH 4 with 1M HCl. This portion is extracted with DCM (2×4 ml) and the organic extracts are combined, passed through a phase separation cartridge, and concentrated in vacuo. The resulting solid is dissolved in ethyl acetate (2 ml) and triturated with iso-hexane (7 ml) to yield the titled compound as a white solid. (MH+400)

1. stirringthe reaction mixture is stirred at room temperature for 2.5 hours
2. customThe resulting mixture is passed through a phase separation cartridge
3. extractionThis portion is extracted with DCM (2×4 ml)
4. custompassed through a phase separation cartridge
5. concentrationconcentrated in vacuo
6. dissolutionThe resulting solid is dissolved in ethyl acetate (2 ml)
7. customtriturated with iso-hexane (7 ml)