HRID333812

反应详情

EQUATION

反应方程式

HRID 333812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooled down to r.t.
  2. extractionextracted twice with water
  3. additionThe combined aqueous phases were treated with concentrated aqueous HCl until pH 3 (16 ml)
  4. filtrationAfter 10 min the solid was filtered
  5. washwashed with water
  6. customdried under high vacuum