反应详情

温度

0 °C

To a solution of the above crude ethyl 3-(3-fluoro-4-(pyrrolo[2,1-f][1,2,4]triazin-4-yloxy)phenylamino)-3-oxopropanoate (180 mg) in ethanol (10 mL) at 0° C. was added 1 N aq NaOH solution (10 mL). After stirring at 0° C. for 3 h, the reaction was washed with 20 mL of EtOAc. The EtOAc layer was back-extracted with 20 mL of 1 N aq NaOH solution. The combined aqueous solution was acidified to pH 5 with 1 N aq HCl solution. The aqueous layer was extracted with EtOAc (3×30 mL). The combined organic extracts were dried over anhydrous Na2SO4 and concentrated in vacuo to give the crude acid which was used without further purification (150 mg). MS(ESI+) m/z 331.1 (M++H)+.

1. washthe reaction was washed with 20 mL of EtOAc
2. extractionThe EtOAc layer was back-extracted with 20 mL of 1 N aq NaOH solution
3. extractionThe aqueous layer was extracted with EtOAc (3×30 mL)
4. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo