Reaktion #8731

Reaktionsgleichung

2-((R)-1-Methyl-pyrrolidin-3-yloxy)-4-nitrobenzotrifluoride

hydrogen

magnesium sulfate

→

product

3-((R)-1-Methyl-pyrrolidin-3-yloxy)-4-trifluoromethyl-phenylamine

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthen filtered through a pad of Celite
2. 2
   WaschenThe filter cake was rinsed with ethyl acetate (2×25 ml)
3. 3
   Sonstigethe filtrate was evaporated under reduced pressure to an oil
4. 4
   SonstigeThis oil was evaporated twice for dichloromethane (50 ml)
5. 5
   Sonstigeto remove

Vorschrift

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).

Quelle