反应详情

4.3 mg of 1-methyl-1H-pyrazole-3-carboxylic acid, 6.0 mg of hydroxybenzotriazole and 8.5 mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide monohydrochloride were added to a dimethylformamide (0.5 ml) solution of 15 mg of 4-(2-fluoro-phenoxy)-5-(6-methanesulfonyl-pyridin-3-yloxy)-benzene-1,2-diamine obtained in Example 200, and the reaction liquid was stirred overnight at room temperature. The reaction liquid was diluted with chloroform, washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and 3 mg of p-toluenesulfonic acid was added to the resulting residue, and the reaction liquid was stirred at 120° C. for 2 hours. The reaction liquid was diluted with ethyl acetate, washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=15/1) to obtain the entitled compound as a white solid.

1. customthe reaction liquid
2. customThe reaction liquid
3. washwashed with water
4. dry with materialdried with anhydrous sodium sulfate
5. customThe solvent was evaporated away under reduced pressure, and 3 mg of p-toluenesulfonic acid
6. additionwas added to the resulting residue
7. customthe reaction liquid
8. stirringwas stirred at 120° C. for 2 hours
9. customThe reaction liquid
10. washwashed with water
11. dry with materialdried with anhydrous sodium sulfate
12. customThe solvent was evaporated away under reduced pressure
13. customthe resulting residue was purified
14. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=15/1)