HRID50052

反应详情

EQUATION

反应方程式

HRID 50052 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. temperaturerefluxed for 30 minutes
  2. concentrationIt is concentrated under vacuum
  3. additionacidified to pH 3 by the addition of 2 N HCl solution
  4. customthe precipitate formed
  5. filtrationis filtered off