HRID330832
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
3.44 mL (45.8 mmol) 1-propanol are added to 3.42 g (30.5 mmol) KOtBu in 18 mL DMF at 0° C. After stirring the solution for 10 min at rt, 1.80 g (7.63 mmol) 4-fluoro-1-iodo-2-methylbenzene are added and the mixture is stirred at 80° C. for 3 h. The reaction is quenched by the addition of sat. aq. NH4Cl solution and extracted with EtOAc (2×). The combined organic layers are washed with sat. aq. NH4Cl solution and brine, dried over sodium sulphate and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, heptane/EtOAc 9/1).
WORKUP
后处理
- stirringthe mixture is stirred at 80° C. for 3 h
- customThe reaction is quenched by the addition of sat. aq. NH4Cl solution
- extractionextracted with EtOAc (2×)
- washThe combined organic layers are washed with sat. aq. NH4Cl solution and brine
- dry with materialdried over sodium sulphate
- customthe solvent is removed in vacuo
- customThe crude product is purified by column chromatography (silica gel, heptane/EtOAc 9/1)