反应详情

温度

100 °C

To a solution of 4-bromo-3,5-dimethylphenol (700 mg) in N,N-dimethylformamide (7 mL) is added Cs2CO3 (1.7 g) and 1-oxa-6-thiaspiro[2.5]octane (586 mg). The mixture is stirred for 12 hour at 100° C. The mixture is diluted with water and extracted twice with ethyl acetate. The combined organic phases are washed with water and brine, dried (MgSO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 99:1→60:40) to give the title compound. Yield: 986 mg; LC (method 7): tR=1.14 min; Mass spectrum (ESI+): m/z=348 [M+NH4]+.

1. extractionextracted twice with ethyl acetate
2. washThe combined organic phases are washed with water and brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 99:1→60:40)