反应详情

To a solution of 5-fluoroindoline (1.0 g, 7.30 mmol) and N-Boc-4-piperidone (1.60 g, 7.50 mmol) in tetrahydrofuran (10.0 mL) was added sodium triacetoxyborohydride (1.80 g, 7.50 mmol). After stirring for 3 hours at room temperature, to the mixture were added saturated sodium bicarbonate water and ethyl acetate, and the aqueous layer was extracted with ethyl acetate. The organic layer was washed with water and brine, and then dried over sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified with silica gel column (chloroform/methanol=98/2 to 90/10) to give a Boc derivative of the title compound. MS (ESI+) 321 (M++1, 100%)

1. extractionthe aqueous layer was extracted with ethyl acetate
2. washThe organic layer was washed with water and brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe obtained residue was purified with silica gel column (chloroform/methanol=98/2 to 90/10)