反应详情

To a solution of 5-chloro-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid hydrazide (Preparation 10—route 2, 0.100 g, 0.48 mmol) in DMF (4 mL) was added HOBt (0.064 g, 0.48 mmol), EDCI (0.110 g, 0.58 mmol), DIPEA (200 μL, 0.96 mmol) and piperonylic acid (0.079 g, 0.48 mmol). The reaction mixture was stirred at rt for 16 h. The reaction mixture was poured into water (75 mL) and extracted with ethyl acetate (2×150 mL). The combined organic extract was washed with saturated sodium chloride (75 mL), dried (MgSO4) and concentrated in vacuo to give a solid. The solid obtained was purified by recrystallisation from methanol to give the title compound. m/z (ES+)=359 [M+H]+; RT=2.92 min.

1. extractionextracted with ethyl acetate (2×150 mL)
2. extractionThe combined organic extract
3. washwas washed with saturated sodium chloride (75 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give a solid
7. customThe solid obtained
8. customwas purified by recrystallisation from methanol