HRID729460
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was cooled to RT
- washwashed Et2O (2×10) mL
- filtrationThe solid was filtered
- washwashed with water
- customThe solid was dried under high vacuum