HRID330832

反应详情

EQUATION

反应方程式

HRID 330832 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringthe mixture is stirred at 80° C. for 3 h
  2. customThe reaction is quenched by the addition of sat. aq. NH4Cl solution
  3. extractionextracted with EtOAc (2×)
  4. washThe combined organic layers are washed with sat. aq. NH4Cl solution and brine
  5. dry with materialdried over sodium sulphate
  6. customthe solvent is removed in vacuo
  7. customThe crude product is purified by column chromatography (silica gel, heptane/EtOAc 9/1)