反应 #48530

ord-4af642cd877e42d0a2406a3765dfc027

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    workup.ADDITIONwas added to the mixture over a period of one hour
  3. 3
    温度to reflux for 10 hours
  4. 4
    温度cooled
  5. 5
    workup.DISTILLATIONthe separated organic layer was distilled

实验过程

A mixture of 2,4-dichlorophenol (105 g, 0.64 mol), 1,2-dibromoethane (157 g, 0.84 mol) and water (500 mL) was heated at reflux, during which time a solution of sodium hydroxide (28.0 g, 0.70 mol) in water (125 mL) was added to the mixture over a period of one hour. The solution was allowed to reflux for 10 hours, cooled and the separated organic layer was distilled to give 1-bromo-2-(2,4-dichlorophenoxy)ethane (106 g, yield 62%). 1HNMR (CDCl3) δ 7.37 (d, 1H, J=2.4 Hz), 7.19 (dd, 1H, J1=8.8 J2=2.4 Hz), 6.88 (d, 1H, J=8.8 Hz), 4.31 (t, 3H, J=6.4 Hz), 3.65 (t, 3H, J=6.4 Hz).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07745629B2uspto-grants-2010_06