Реакция #710541

ord-668c4c329c744e1180d717e9b074ff4b

Растворители

Условия реакции

Температура
100°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияthe reaction extracted with EtOAc
  2. 2
    Промывкаwashed with brine
  3. 3
    Сушкаdried with Na2SO4
  4. 4
    Концентрированиеconcentrated
  5. 5
    Другоеpurified by silica gel column chromatography (0-50% DCM in cyclohexane)

Методика

To a mixture of C-(4-bromo-phenyl)-N-(3-chloro-phenyl)-methanesulfonamide (0.61 g, 1.68 mmol) and K2CO3 (464 mg, 3.4 mmol) in dimethylformamide (5 mL) was added 1-iodo-2-methylpropane (584 μL, 5.0 mmol). The mixture was heated at 100° C. in microwave reactor for 3 hours. Water was added and the reaction extracted with EtOAc, washed with brine, dried with Na2SO4, concentrated and purified by silica gel column chromatography (0-50% DCM in cyclohexane) to give C-(4-bromo-phenyl)-N-(3-chloro-phenyl)-N-isobutyl-methanesulfonamide (423 mg, 1.0 mmol, 60%). LCMS (m/z, Method A) ES+ 415.8 [M+1]+.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09302985B2uspto-grants-2016_04