HRID729460

反应详情

EQUATION

反应方程式

HRID 729460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 2-(4-hydroxypiperidin-1-yl)pyrimidine-5-carbonitrile (2 g, 9.79 mmol), sodium azide (0.955 g, 14.69 mmol) and ammonium chloride (1.048 g, 19.59 mmol) in DMF (24.48 mL) was heated at 130° C. for 1 h. The mixture was cooled to RT, diluted with 1N NaOH (5 mL), washed Et2O (2×10) mL. The aqueous layer was acidified to pH about 1 with 2 N HCl and placed in the refrigerator for 1 h. The solid was filtered and washed with water followed by Et2O. The solid was dried under high vacuum to afford the title compound.

WORKUP

后处理

  1. temperatureThe mixture was cooled to RT
  2. washwashed Et2O (2×10) mL
  3. filtrationThe solid was filtered
  4. washwashed with water
  5. customThe solid was dried under high vacuum