HRID237555
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
To a mixture of 4-bromo-3,5-dimethylphenol (625 mg) and Cs2CO3 (5 g) in N,N-dimethylformamide (10 mL) is added 5,5-dimethyl-[1,3,2]dioxathiane-2-oxide (467 mg). The mixture is stirred for 12 hours at 100° C. and then partitioned between water and ethyl acetate. The organic phase is washed with brine and dried (MgSO4). The solvent is evaporated and the residue is purified by HPLC on reversed phase to give the title compound. Yield: 251 mg; LC (method 7): tR=1.16 min; Mass spectrum (ESI+): m/z=287 [M+H]+.
WORKUP
后处理
- custompartitioned between water and ethyl acetate
- washThe organic phase is washed with brine
- dry with materialdried (MgSO4)
- customThe solvent is evaporated
- customthe residue is purified by HPLC on reversed phase