HRID2244352

反应详情

EQUATION

反应方程式

HRID 2244352 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

A mixture of 2-chloro-5-fluoropyridine-6-carboxylic acid (2.00 g, 11.4 mmol), 41% aq. methylamine solution (8 mL) and 1,4-dioxane (8 mL) was heated at 125° C. under microwave irradiation for 60 min. After cooling, volatile material was distilled off, and the residue was dissolved in water (20 mL) and acidified to pH 3 by addition of 37% aq. hydrochloric acid solution. The precipitate was collected by filtration to produce the title compound (1.85 g, 87%). Light yellow solid, MS (ISP): 185.1 (M−H)−.

WORKUP

后处理

  1. temperatureAfter cooling
  2. distillationvolatile material was distilled off
  3. dissolutionthe residue was dissolved in water (20 mL)
  4. additionacidified to pH 3 by addition of 37% aq. hydrochloric acid solution
  5. filtrationThe precipitate was collected by filtration