反应详情

温度

120 °C

In a microwave vial Cs2CO3 (5.4 g) is added to a solution of 5,5-dimethyl-[1,3,2]dioxathiane 2-oxide (500 mg) and 4-bromo-3,5-dimethylphenol (670 mg) in N,N-dimethylformamide (5 mL). The vial is sealed and the mixture is heated to 120° C. for 12 hours. The mixture is partitioned between ethyl acetate and water. The organic phase is washed three times with 2 M aqueous NaOH and with brine. After drying (MgSO4) and concentration the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 99:1→50:50) to give the title compound. Yield: 372 mg; LC (method 7): tR=1.17 min; Mass spectrum (ESI+): m/z=287 [M+H]+.

1. customThe vial is sealed
2. customThe mixture is partitioned between ethyl acetate and water
3. washThe organic phase is washed three times with 2 M aqueous NaOH
4. customAfter drying
5. concentration(MgSO4) and concentration the residue
6. customis chromatographed on silica gel (cyclohexane/ethyl acetate 99:1→50:50)