反应详情

To a solution of the compound obtained in step 3 (200 mg), triethylamine (313 μL) and 1-(hydroxyacetyl)piperidine-4-carboxylic acid (101 mg) in DMF (4.5 mL) was added DEPC (87 mg), and the mixture was stirred overnight at room temperature. To the reaction mixture was added water, and the resultant product was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogen carbonate solution, 1N hydrochloric acid and brine and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH Chromatorex) (solvent gradient; 40→95% ethyl acetate/hexane) to give the title compound (135 mg, 49%) as a white crystal powder.

1. extractionthe resultant product was extracted with ethyl acetate
2. washThe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution, 1N hydrochloric acid and brine
3. customdried
4. customthe solvent was evaporated under reduced pressure
5. customThe obtained residue was purified by silica gel column chromatography (NH Chromatorex) (solvent gradient; 40→95% ethyl acetate/hexane)