反应 #1857545

ord-d28a0637a7d54976a9f91daca538b9aa

反应方程式

CC(=O)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone
BrBr
bromine
[Na+].[OH-]
NaOH
O=C(CBr)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
2-bromo-1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONAfter completion of the addition the mixture
  2. 2
    其他The organic layer was separated
  3. 3
    萃取extracted twice with MTBE
  4. 4
    洗涤the combined organic phases were washed with sat. NaHCO3 solution (1×) and brine (2×)
  5. 5
    其他The solvent was evaporated

实验过程

1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone (1000 g) was dissolved in MTBE (5000 mL) and a solution of bromine (563 g) in glacial acetic acid (400 mL) was added dropwise at room temperature. After completion of the addition the mixture was stirred for 1 h at room temperature and the pH was adjusted to 7-8 by addition of 10% NaOH solution. The organic layer was separated, extracted twice with MTBE and the combined organic phases were washed with sat. NaHCO3 solution (1×) and brine (2×). The solvent was evaporated and the crude product was used directly in the next step.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09247747B2uspto-grants-2016_02