반응 #1983

반응 방정식

compound

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

diphenylphosphoryl azide

trimethyl amine

t-butanol

→

title compound

수율 96.7%

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

수율 96.7%

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux under N2 for 24 hours
3. 3
   농축The mixture was concentrated to dryness
4. 4
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride
5. 5
   세척The solution was washed with satd
6. 6
   농축NaHCO3 and water, then concentrated
7. 7
   기타The residue was chromatographed on silica gel

실험 절차

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.

출처