HRID1971830
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
- 50 °C
PROCEDURE
实验过程
To a solution of 1,2-dichloro-4-iodobenzene (5.44 g, 20 mmol) in DMF (60 ml) was added Bu4NCl (5.56 g, 20 mmol), propenol (4.64 g, 80 mmol), Pd(OAc)2 (224 mg, 1 mmol) and NaHCO3 (10.0 g, 120 mmol) successively at room temperature. The mixture was heated at 50° C. for 12 hour. After cooling to the room temperature, the mixture was poured into ice-water, extracted with DCM three times. The combined organic layers were washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography using PE/EA (20/1) as eluent to afford the title compound (2.01 g, yield 49.8%).
WORKUP
后处理
- temperatureAfter cooling to the room temperature
- extractionextracted with DCM three times
- washThe combined organic layers were washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography