反応 #78330

反応方程式

di-tert-butyl carbonate

triethylamine

water

isonipecotic acid

→

expected product

収率 95.8%

1-tert-Butoxycarbonyl-4-carboxypiperidine

収率 95.8%

溶媒

dioxane

反応条件

後処理

1. 1
   温度refluxed for 30 minutes
2. 2
   濃縮It is concentrated under vacuum
3. 3
   workup.ADDITIONacidified to pH 3 by the addition of 2 N HCl solution
4. 4
   その他the precipitate formed
5. 5
   ろ過is filtered off

実験手順

8.6 g of triethylamine and 20 ml of water are added to a solution of 10 g of isonipecotic acid in 100 ml of dioxane and the mixture is heated to 60° C. 20.25 g of di-tert-butyl carbonate are then added dropwise and the mixture is stirred for 1 hour at 60° C. and refluxed for 30 minutes. It is concentrated under vacuum, the residue is taken up with water and acidified to pH 3 by the addition of 2 N HCl solution and the precipitate formed is filtered off to give 17 g of the expected product.

出典