HRID333812
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
- 125 °C
PROCEDURE
实验过程
2-Chloro isonicotinic acid (9.45 g) and benzyl alcohol (12.977 g) were dissolved in NMP (180 mL), and treated with tBuOK (20.2 g) between 10-25° C. The reaction mixture was then stirred at 125° C. (Bath-temperature) for 6 h, cooled down to r.t., poured into water (1500 ml) and extracted twice with water. The combined aqueous phases were treated with concentrated aqueous HCl until pH 3 (16 ml). After 10 min the solid was filtered, washed with water and dried under high vacuum, to give the title compound as an off-white solid (9.8 g). MS (m/e)=228.1 (M−H).
WORKUP
后处理
- temperaturecooled down to r.t.
- extractionextracted twice with water
- additionThe combined aqueous phases were treated with concentrated aqueous HCl until pH 3 (16 ml)
- filtrationAfter 10 min the solid was filtered
- washwashed with water
- customdried under high vacuum