HRID241759

反应详情

EQUATION

反应方程式

HRID 241759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 3-[2-(3,5-dichloro-pyrid-2-yl)-acetylamino]-pyrazine-2-carboxylic acid methyl ester (Example 1.1) (5.78 g) and potassium carbonate (2.4 g) in dry N,N-dimethylformamide (100 ml) was heated to 100° C. for 2 hours. The reaction mixture was cooled to ambient temperature and concentrated. The residue was triturated with diethyl ether and the organic phase decanted. The solid was dissolved in water and pH value adjusted to pH 5 by addition of aqueous hydrochloric acid (2M). The aqueous phase was concentrated. The residue was dissolved in methanol, the insoluble salts were removed by filtration and the filtrate was concentrated to give Compound No. A1 of Table A (4.9 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to ambient temperature
  2. concentrationconcentrated
  3. customThe residue was triturated with diethyl ether
  4. customthe organic phase decanted
  5. dissolutionThe solid was dissolved in water
  6. additionpH value adjusted to pH 5 by addition of aqueous hydrochloric acid (2M)
  7. concentrationThe aqueous phase was concentrated
  8. dissolutionThe residue was dissolved in methanol
  9. customthe insoluble salts were removed by filtration
  10. concentrationthe filtrate was concentrated
  11. customto give Compound No