反应详情

温度

80 °C

A mixture of 1,1-dimethylethyl 4-{3-[6-amino-2-(methyloxy)-3-pyridinyl]-3-oxopropyl}-1-piperidinecarboxylate (step 3, 300 mg, 0.825 mmol) and N-chlorosuccinimide (115.7 mg, 0.866mmol) in N,N-dimethylformamide (5 ml) was stirred at 80° C. for 4 h. After cooling to room temperature, the mixture was diluted with diethylether (150 ml), washed with water (50 ml×2) and brine (150 ml), and dried over magnesium sulfate. Removal of solvent gave a brown oil, which was chromatographed on a column of silica gel eluting with ethyl acetate/hexane (2:1) to afford 182 mg (56%) of the title compound as a colorless oil.

1. temperatureAfter cooling to room temperature
2. washwashed with water (50 ml×2) and brine (150 ml)
3. dry with materialdried over magnesium sulfate
4. customRemoval of solvent
5. customgave a brown oil, which
6. customwas chromatographed on a column of silica gel eluting with ethyl acetate/hexane (2:1)