反应详情

After dissolving 1.09 g of 4-(2-fluorophenoxymethyl)piperidine in 15 ml of methanol, 1.53 ml of titanium (IV) tetraisopropoxide and 400 mg of 2-acetyl-3-methoxypyrazine [CAS No. 56343-40-9] were added and the mixture was stirred overnight at room temperature. The reaction solution was cooled on ice, 148 mg of sodium borohydride was added and the mixture was stirred for 5 hours at room temperature. Water and ethyl acetate were added to the reaction solution and the mixture was filtered with celite. The filtrate was extracted with ethyl acetate and the extract was washed with saturated brine and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by NH silica gel column chromatography (solvent: n-hexane/ethyl acetate) to obtain the title compound (100 mg, 11% yield).

1. addition56343-40-9] were added
2. additionwas added
3. stirringthe mixture was stirred for 5 hours at room temperature
4. filtrationthe mixture was filtered with celite
5. extractionThe filtrate was extracted with ethyl acetate
6. washthe extract was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. customthe residue was purified by NH silica gel column chromatography (solvent: n-hexane/ethyl acetate)