反应详情

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0 °C

To a trifluoroacetic acid (11 mL) solution of 2-amino-N-(6-benzyloxy-benzofuran-2-ylmethyl)-6-methoxymethyl-nicotinamide (557 mg, 1.33 mmol) described in Example 4 was added thioanisole (626 μL, 5.35 mmol) at 0° C., which was stirred at 0° C. for 3 hours. To the reaction solution were added sodium bicarbonate and water at 0° C. followed by extraction with ethyl acetate and tetrahydrofuran. The organic layer was washed with sat. NaCl followed by drying over anhydrous magnesium sulfate and filtering. The filtrate was concentrated under a reduced pressure and the residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=10:1) to obtain the title compound (331 mg, 76%) as a white solid.

1. extractionfollowed by extraction with ethyl acetate and tetrahydrofuran
2. washThe organic layer was washed with sat. NaCl
3. dry with materialby drying over anhydrous magnesium sulfate
4. filtrationfiltering
5. concentrationThe filtrate was concentrated under a reduced pressure
6. customthe residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=10:1)