HRID23961

反应详情

EQUATION

反应方程式

HRID 23961 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirring solution of ethyl pyridine-2-acetate (12.6 g, 76.3 mmol) in acetic acid (19 mL) at 5° C. was added a solution of sodium nitrite (6.05 g, 87.7 mmol) in water (12 mL) at a rate sufficient to maintain the internal temperature below 15° C. After complete addition and an additional 30 min, an additional 30 mL of water was added. The resulting white precipitate was filtered, washed with water, saturated aqueous NaHCO3, and again with water. The solid was then dried under vacuum to give 14.1 g (95%) of the title compound.

WORKUP

后处理

  1. temperatureto maintain the internal temperature below 15° C
  2. additionAfter complete addition
  3. filtrationThe resulting white precipitate was filtered
  4. washwashed with water, saturated aqueous NaHCO3
  5. customThe solid was then dried under vacuum