HRID610685

反应详情

EQUATION

反应方程式

HRID 610685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phenol (3.10 g, 33 mmol), 1,7-dibromoheptane (7.74 g, 30 mmol) and NaOH (1.34 g, 33 mmol) were refluxed in EtOH (40 mL) for 30 h. After cooling to room temperature, water (150 mL) was added and the mixture was extracted with ethyl acetate (4×50 mL). The organic phase was washed with water (50 mL) and brine (50 mL), and the mixture was dried over Na2SO4. After evaporation of solvent, the residue was purified by Kugelrohr distillation to give 7-phenoxyheptyl bromide (2.46 g, 30%), bp 126-130° C./0.10 torr, 1H-NMR: 1.2-1.9 (m, 10H), 3.36 (t, 2H), 3.91 (t, 2H), 6.7-7.2 (m, 5H).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate (4×50 mL)
  2. washThe organic phase was washed with water (50 mL) and brine (50 mL)
  3. dry with materialthe mixture was dried over Na2SO4
  4. customAfter evaporation of solvent
  5. distillationthe residue was purified by Kugelrohr distillation