HRID1250727

反应详情

EQUATION

反应方程式

HRID 1250727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 7.18 g (71 mmol) of 4-hydroxypiperidine in 100 ml dimethylformamide are added first 19.6 g (142 mmol) of powdered potassium carbonate and then 19.8 9 (71 mmol) of tritylchloride. The mixture is stirred for 22 hours at ambient temperature, diluted with ethyl acetate to twice the volume, washed with water and saturated saline solution, dried with magnesium sulphate and concentrated by evaporation. The residue is recrystallised from ethyl acetate/petroleum ether (1:4, v:v). 17.65 g (72.4% of theory) of 4-hydroxy-N-tritylpiperidine are obtained as colourless crystals, melting point 157-158° C.

WORKUP

后处理

  1. washwashed with water and saturated saline solution
  2. dry with materialdried with magnesium sulphate
  3. concentrationconcentrated by evaporation
  4. customThe residue is recrystallised from ethyl acetate/petroleum ether (1:4, v:v)