반응 #58640

ord-5e33a3e3b9f64f40bdf888361e641c1b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타crushed activated molecular sieves (4 g)
  2. 2
    workup.STIRRINGAfter stirring at room temperature for 1 h
  3. 3
    workup.ADDITIONCELITE diatomaceous earth (4 g) was added
  4. 4
    여과The resulting mixture was filtered through a silica gel pad, which
  5. 5
    세척was washed with ether (2×50 mL)
  6. 6
    농축The filtrate was concentrated to dryness
  7. 7
    기타azeotroped with toluene

실험 절차

To a solution of 3-(2,4-dichlorophenyl)-2-(4-chorophenyl)propanol (Step B, 0.89 g, 2.8 mmol) in 20 mL CH2Cl2 was added crushed activated molecular sieves (4 g). After stirring at room temperature for 10 min, pyridinium chlorochromate (0.90 g, 4.2 mmol) was added. After stirring at room temperature for 1 h, CELITE diatomaceous earth (4 g) was added followed by 100 mL ether. The resulting mixture was filtered through a silica gel pad, which was washed with ether (2×50 mL). The filtrate was concentrated to dryness and azeotroped with toluene to give the title compound, which was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07423067B2uspto-grants-2008_09