反应 #1983

反应方程式

compound

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

diphenylphosphoryl azide

trimethyl amine

t-butanol

→

title compound

收率 96.7%

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

收率 96.7%

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux under N2 for 24 hours
3. 3
   浓缩The mixture was concentrated to dryness
4. 4
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride
5. 5
   洗涤The solution was washed with satd
6. 6
   浓缩NaHCO3 and water, then concentrated
7. 7
   其他The residue was chromatographed on silica gel

实验过程

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.

来源