HRID1360690
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
- 90 °C
PROCEDURE
实验过程
To a solution of 4-bromo-2,6-difluorobenzyl methanesulfonate (from Step A above) in DMF (400 mL) was added LiBr (28.8 g, 335 mmol) and heated to 90° C. for 45 minutes. The reaction was cooled to room temperature and diluted with EtOAc. The organic layer was washed with water (5×), brine (2×) dried over MgSO4, and concentrated in vacuo to yield a brown oil. The crude residue was purified via silica gel column chromatography (CH2Cl2/hexanes) to yield the title compound (24 g).
WORKUP
后处理
- temperatureThe reaction was cooled to room temperature
- washThe organic layer was washed with water (5×), brine (2×)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customto yield a brown oil
- customThe crude residue was purified via silica gel column chromatography (CH2Cl2/hexanes)