HRID2197484
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was cooled to ambient temperature
- concentrationconcentrated
- customThe residue was triturated with diethyl ether
- customthe organic phase decanted
- dissolutionThe solid was dissolved in water
- additionpH value adjusted to pH 5 by addition of aqueous hydrochloric acid (2M)
- concentrationThe aqueous phase was concentrated
- dissolutionThe residue was dissolved in methanol
- customthe insoluble salts were removed by filtration
- concentrationthe filtrate was concentrated
- customto give Compound No