反应详情

7.7 mg of pyrazine-2-carboxylic acid and 20 mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide monohydrochloride were added to a pyridine (1 ml) solution of 15 mg of 4,5-bis(pyridin-3-yloxy)-benzene-1,2-diamine obtained in Example 1 (step 3), and the reaction liquid was stirred overnight at room temperature. The reaction liquid was diluted with ethyl acetate, washed with saturated sodium bicarbonate solution, water and saturated saline in order, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was suspended in 1 ml of phosphorus oxychloride, and the reaction liquid was stirred overnight at 100° C. Phosphorus oxychloride was evaporated away under reduced pressure, and this was diluted with ethyl acetate, washed with saturated sodium bicarbonate solution and saturated saline in order, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=15/1+0.1% aqueous ammonia) to obtain the entitled compound as a yellow solid.

1. customthe reaction liquid
2. customThe reaction liquid
3. washwashed with saturated sodium bicarbonate solution, water and saturated saline in order
4. dry with materialdried with anhydrous sodium sulfate
5. customThe solvent was evaporated away under reduced pressure
6. customthe reaction liquid
7. stirringwas stirred overnight at 100° C
8. customPhosphorus oxychloride was evaporated away under reduced pressure
9. additionthis was diluted with ethyl acetate
10. washwashed with saturated sodium bicarbonate solution and saturated saline in order
11. dry with materialdried with anhydrous sodium sulfate
12. customThe solvent was evaporated away under reduced pressure
13. customthe residue was purified
14. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=15/1+0.1% aqueous ammonia)