반응 #157757

ord-8bcaa7ff2ea546a39b6e4c98f3640ab5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature for 18 hours
  2. 2
    추출followed by extraction with chloroform
  3. 3
    건조The organic layer was dried over anhydrous magnesium sulfate
  4. 4
    여과filtered
  5. 5
    기타The solvent was then evaporated under reduced pressure
  6. 6
    기타The residue was purified by silica gel column chromatography (chloroform only)

실험 절차

Oxone(R) (20.3 g) was added to a solution of 4-bromo-2-chloro-1-(cyclopropylsulfanyl)benzene obtained in Reference Example 5-22 (964 mg) in tetrahydrofuran (20 mL)-methanol (20 mL)-water (10 mL), and the mixture was stirred at room temperature for one day. Oxone(R) (6.8 g) was further added and the mixture was stirred at room temperature for 18 hours. Water was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform only) to give the title compound as a pale yellow amorphous (597 mg, 55%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822503B2uspto-grants-2014_09