HRID1269743

反应详情

EQUATION

反应方程式

HRID 1269743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 4N-aqueous sodium hydroxide solution (15 ml) was added to a solution of ethyl 1-benzyl-3-piperidinecarboxylate (7.00 g, 28.3 mmol) in a mixture of tetrahydrofuran (30 ml) and 1,4-dioxane (30 ml), and the resulting mixture was stirred at room temperature for 4 hours. After a 4N-aqueous sodium hydroxide solution (15 ml) was added again, the resulting mixture was stirred overnight at room temperature. After completion of the reaction, the reaction solution was neutralized by the addition of 2N-hydrochloric acid (15 ml) under ice-cooling and the resulting mixture was subjected to azeotropic concentration with toluene. The residue was suspended in ethanol, followed by filtration, and the filtrate was concentrated to obtain 1-benzyl-3-piperidinecarboxylic acid (6.3 g, 100%).

WORKUP

后处理

  1. stirringthe resulting mixture was stirred overnight at room temperature
  2. customAfter completion of the reaction
  3. temperaturecooling
  4. concentrationthe resulting mixture was subjected to azeotropic concentration with toluene
  5. filtrationfollowed by filtration
  6. concentrationthe filtrate was concentrated