HRID50834

反应详情

EQUATION

反应方程式

HRID 50834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution 2,6-difluoronicotinic acid (7.4 g, 0.046 mmol) and SOCl2 (20 mL) in 1,2-dichloroethane (60 mL) containing DMF (1 drop) is heated under reflux for 4 h, then concentrated to dryness under reduced pressure. The residue is dissolved in Et2O (100 mL), cooled to 0° C., and treated dropwise with concentrated ammonia (10.0 mL, 0.17 mmol). After 10 min the solution is washed with aqueous NaHCO3 and worked up to give 2,6-difluoronicotinamide (5.61 g, 76%). 1H NMR (CDCl3) a 8.70 (1H, dd, J=9.6, 8.3 Hz), 7.00 (1H, ddd, J=8.3, 2.9, 1.1 Hz), 6.71, 6.55 (1H, 1H, 2 brs)

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 4 h
  3. concentrationconcentrated to dryness under reduced pressure
  4. dissolutionThe residue is dissolved in Et2O (100 mL)
  5. washAfter 10 min the solution is washed with aqueous NaHCO3