反应详情

温度

60 °C

A mixture of 4-bromo-triazole (0.30 g), toluene-4-sulfonic acid tetrahydro-pyran-4-yl ester (0.52 g), cesium carbonate (1.00 g), and N,N-dimethylformamide (7 mL) was stirred at 60° C. overnight. After cooling to ambient temperature, water was added and the resulting mixture was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4), and concentrated. The residue was triturated with cyclohexane/diethyl ether to afford the title compound as a colorless solid. Yield: 0.26 g (55% of theory); LC (method 3): tR=2.75 min; Mass spectrum (ESI+): m/z=231/233 (Br) [M+H]+.

1. temperatureAfter cooling to ambient temperature
2. extractionthe resulting mixture was extracted with ethyl acetate
3. washThe combined organic extracts were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe residue was triturated with cyclohexane/diethyl ether