反应详情

A mixture of N-(3-bromo-4-fluorobenzyl)tetrahydro-2H-thiopyran-4-amine (1.72 g), 1-methyl-1H-imidazole-4-carboxylic acid (0.71 g), EDC.HCl (1.63 g), HOBt (0.87 g), dimethylformamide (30 mL) and triethylamine (1.8 mL) was stirred overnight at room temperature. The solvent was distilled off under reduced pressure and after extraction with ethyl acetate, the extract was washed with a saturated aqueous solution of sodium hydrogencarbonate and saturated saline, and dried over anhydrous magnesium sulfate. After filtering off the desiccant, the solvent was concentrated. The residue was purified by column chromatography (NH silica gel cartridge; ethyl acetate) to give the titled compound (1.55 g).

1. distillationThe solvent was distilled off under reduced pressure
2. extractionafter extraction with ethyl acetate
3. washthe extract was washed with a saturated aqueous solution of sodium hydrogencarbonate and saturated saline
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationAfter filtering off the desiccant
6. concentrationthe solvent was concentrated
7. customThe residue was purified by column chromatography (NH silica gel cartridge; ethyl acetate)