반응 #1857542

ord-b37ba3fbf1c34340a361306fe0dd4206

반응 방정식

[Cl-].[NH4+]
NH4Cl
[H-].[Na+]
sodium hydride
CC(=O)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone
C[S+](C)C.[I-]
trimethylsulfonium iodide
CC1(c2ccc(Oc3ccc(Cl)cc3)cc2Cl)CO1
desired compound
CC1(c2ccc(Oc3ccc(Cl)cc3)cc2Cl)CO1
2-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-methyloxirane

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added carefully
  2. 2
    추출The mixture was extracted with MTBE (3×)
  3. 3
    세척the combined organic phases were washed with water
  4. 4
    기타dried
  5. 5
    기타evaporated

실험 절차

DMSO (150 mL) was added dropwise to a mixture of sodium hydride (22 g) in THF (600 mL). After completion of the addition a solution of trimethylsulfonium iodide (171 g) in DMSO (300 mL) was added slowly at 5° C. whereupon a solution of 1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone (107 g) in DMSO (300 mL) was added carefully. The mixture was stirred for 1 h at room temperature and dil. NH4Cl solution was added. The mixture was extracted with MTBE (3×) and the combined organic phases were washed with water, dried and evaporated to obtain the desired compound that was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09247746B2uspto-grants-2016_02