HRID1386730
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
PROCEDURE
实验过程
To a solution of 5.0 g (24.0 mmol) of 2,6 difluoro-4-bromophenol in 20 ml of DMF at rt was added 5 g (36.0 mmol) of K2CO3 followed by 4.5 g (26.3 mmol) of benzyl bromide. The mixture was stirred for 12 h, diluted with H2O, the organic phase washed with sat'd NaCl, and the aqueous phase was then extracted 3× with CH2Cl2. The combined organic layers were dried over Na2SO4 and concentrated. Flash chromatography with a gradient of 0-15% ethyl acetate/hexanes (v/v) afforded 6.3 g (88%) of the title compound: 1H NMR (500 MHz) δ 5.17 (s, 21), 7.06-7.11 (2H). 7.34-7.45 (5H).
WORKUP
后处理
- washthe organic phase washed with sat'd NaCl
- extractionthe aqueous phase was then extracted 3× with CH2Cl2
- dry with materialThe combined organic layers were dried over Na2SO4
- concentrationconcentrated