HRID626184

反应详情

EQUATION

反应方程式

HRID 626184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-chloroisonicotinic acid (15 g, 1.0 eq) in 200 mL water at 0° C. was added KOH (40 g, 7.5 eq). Then the reaction mixture was heated to reflux for 36 h., cooled, and 3 N HCl (aq) was added to pH=1˜3. The precipitate was collected by filtration and washed with water to give the product as a white solid (13.1 g, 99% yield). 1H NMR (400 MHz, DMSO-d6) δ 12.80 (brs, 2H), 7.47 (d, J=6.4 Hz, 1H), 6.79 (s, 1H), 6.50 (dd, J=6.8 Hz, 1.6 Hz, 1H).

WORKUP

后处理

  1. temperatureThen the reaction mixture was heated
  2. temperatureto reflux for 36 h.
  3. temperaturecooled
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water