Реакция #90155

ord-6ec5e21cb10749b2bce068c801c9440e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISTILLATIONdistilled water (400 ml)
  2. 2
    ФильтрацияThe precipitated solid was collected by filtration
  3. 3
    Промывкаwashed with distilled water
  4. 4
    Другоеdried
  5. 5
    workup.DISSOLUTIONThe crude product was dissolved in DMA (45 ml)
  6. 6
    workup.ADDITIONdiluted with acetonitrile (20 ml)
  7. 7
    workup.DISTILLATIONdistilled water (18 ml)
  8. 8
    Другоеre-precipitated

Методика

Tert-butyl 6-cyano-2-(2-(4-ethyl-3-iodophenyl)propan-2-yl)-1H-indole-3-carboxylic acid (11 g) was dissolved in Eaton's reagent (200 g) and stirred at room temperature for 30 min. The reaction solution was diluted with acetonitrile (200 ml) and distilled water (400 ml). The precipitated solid was collected by filtration, washed with distilled water, and then dried. The crude product was dissolved in DMA (45 ml), diluted with acetonitrile (20 ml) and distilled water (18 ml), and re-precipitated to obtain the title compound (6.62 g, 70%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09440922B2uspto-grants-2016_09