Реакция #73823

ord-9fb6f5778b0846c0a20c64ea1f2da994

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Промывкаwashed with 1:2 water/brine, water and brine (×2)
  2. 2
    СушкаThe organic phase was dried (MgSO4)
  3. 3
    Фильтрацияfiltered
  4. 4
    Концентрированиеconcentrated

Методика

Sodium hydride (60% dispersion in oil, 128 mg, 3.2 mmol) was placed under N2 then DMSO (5 mL) was added. Trimethylsulfonium iodide (0.66 g, 3.2 mmol) was added as a solid after 15 min, followed after a further 30 min by (4-chloro-phenyl)-(4-iodo-phenyl)-methanone. The mixture was stirred at room temperature for 24 hours then diluted with ethyl acetate and washed with 1:2 water/brine, water and brine (×2). The organic phase was dried (MgSO4), filtered and concentrated to give the title compound (1.01 g, 97%), which was used without further purification. LCMS (PS-A2) Rt 4.07 min [M−H]+ 355.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08541461B2uspto-grants-2013_09