反应详情

温度

40 °C

A mixture of methyl 3-[(dipropylamino)carbonyl]-5-(3-thienyl)benzoate (XLIX, step 3, 0.31 g, 0.88 mmol) in THF/methanol/sodium hydroxide (3/1/1, 5 mL) is stirred at 40 degrees C. for 2 hours. The reaction is cooled to 20-25 degrees C., diluted with water and extracted with ethyl acetate. The aqueous phase is acidified to pH=4 and extracted with ethyl acetate. The organic phase is washed with water and saline, dried over magnesium sulfate and concentrated under reduced pressure to give 3-[(dipropylamino)carbonyl]-5-(3-thienyl)benzoic acid (IX-L), ESI-MS (m/z) [M+H]+=332.

1. temperatureThe reaction is cooled to 20-25 degrees C
2. extractionextracted with ethyl acetate
3. extractionextracted with ethyl acetate
4. washThe organic phase is washed with water and saline
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure