反应详情

A solution of (E)-2-[2-(1H-indazol-3-yl)vinyl]benzoic acid (35 mg, 0.13 mmol) obtained in Step 1 of Example 47 in THF (1.0 mL) was sequentially added with 4-methylmorpholine (29 μL, 0.27 mmol), 2-(aminomethyl)thiophene (23 mg, 0.28 mmol) and EDC (36 mg, 0.19 mmol) and stirred at room temperature for 1.0 hour. The reaction mixture was added with water and ethyl acetate to separate the mixture into organic layer and aqueous layer and the organic layer was concentrated under reduced pressure. The residue was purified by silica gel chromatography (chloroform/methanol=100/0 to 90/10) and the obtained compound was crystallized from a mixed solvent of hexane/ethyl acetate (9/1, 1.0 mL) to obtain Compound 141 (11 mg, 17%).

1. customto separate the mixture into organic layer and aqueous layer
2. concentrationthe organic layer was concentrated under reduced pressure
3. customThe residue was purified by silica gel chromatography (chloroform/methanol=100/0 to 90/10)
4. customthe obtained compound was crystallized from a mixed solvent of hexane/ethyl acetate (9/1, 1.0 mL)