Реакция #1544479

ord-d4f7fabfe22c4a79b24ec12ab94bb75b

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISSOLUTIONdissolved in
  2. 2
    workup.ADDITION, is then added dropwise at -5° C
  3. 3
    ДругоеAfter acidification by means of hydrochloric acid (pH=2), the organic phase is separated off
  4. 4
    Другоеevaporated
  5. 5
    ДругоеThe crude product is recrystallized from acetonitrile

Методика

2-Bromo-5-phenyl-1,3,4-thiadiazole (2.9 g, 12 mmol) is added to a 1-octylmagnesium bromide solution (4.6 g, 24 mmol) in THF (80 ml) under a protective-gas atmosphere, and 1,3-bis(diphenylphosphino)propylnickel(II) chloride (0.15 mmol), dissolved in . . . , is then added dropwise at -5° C. The mixture is subsequently stirred at this temperature for 4 hours. After acidification by means of hydrochloric acid (pH=2), the organic phase is separated off and evaporated. The crude product is recrystallized from acetonitrile.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05847149uspto-grants-1998_12