Reaktion #1537273

Reaktionsgleichung

compound

1-benzyl-3-trifluoromethylpyrrolidine-3-carboxylic acid

diphenylphosphoryl azide

trimethyl amine

t-butanol

→

title compound

Ausbeute 96.7%

1-benzyl-3-(BOC-amino)-3-trifluoromethylpyrrolidine

Ausbeute 96.7%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturat reflux under N2 for 24 hours
3. 3
   EinengenThe mixture was concentrated to dryness
4. 4
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride
5. 5
   WaschenThe solution was washed with satd
6. 6
   EinengenNaHCO3 and water, then concentrated
7. 7
   SonstigeThe residue was chromatographed on silica gel

Vorschrift

A mixture of 1.42 g of the compound from step 454a, 1.71 g of diphenylphosphoryl azide, 12.3 g of t-butanol and 0.627 g of trimethyl amine was heated at reflux under N2 for 24 hours. The mixture was concentrated to dryness, and the residue was dissolved in methylene chloride. The solution was washed with satd. NaHCO3 and water, then concentrated. The residue was chromatographed on silica gel to give 1.73 g of the title compound.

Quelle