Реакция #8731

ord-6bc67ca7fb6f48d4b4d2e9c4d8a61c2c

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Фильтрацияthen filtered through a pad of Celite
  2. 2
    ПромывкаThe filter cake was rinsed with ethyl acetate (2×25 ml)
  3. 3
    Другоеthe filtrate was evaporated under reduced pressure to an oil
  4. 4
    ДругоеThis oil was evaporated twice for dichloromethane (50 ml)
  5. 5
    Другоеto remove

Методика

A solution of 2-((R)-1-Methyl-pyrrolidin-3-yloxy)-4-nitrobenzotrifluoride (7.8 g, 26.9 mmol) in ethyl acetate (50 ml) was treated with 10% platinum on carbon (200 mg) then subjected to 40 psi hydrogen pressure for 3 hrs. The slurry was treated with anhydrous magnesium sulfate (5 g) then filtered through a pad of Celite. The filter cake was rinsed with ethyl acetate (2×25 ml) then the filtrate was evaporated under reduced pressure to an oil. This oil was evaporated twice for dichloromethane (50 ml) to remove trapped ethyl acetate. This gave the product as a clear light brown oil that solidified on standing (6.9 g, 99%): LCMS 249 (M++H).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07091204B2uspto-grants-2006_08