反应详情

2,2-Dimethylpropyl 4-{4-[amino(hydroxyimino)methyl]pyridin-2-yl}piperazine-1-carboxylate (340 mg) obtained in Example 26-1) was dissolved in acetonitrile (2 mL), and 1,1′-thiocarbonyldiimidazole (231 mg) was added thereto and stirred at room temperature for 2 hours. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was dissolved in dimethylformamide (2 mL), and methyl iodide (0.080 mL) and potassium carbonate (198 mg) were added thereto and stirred at room temperature for 1 hour. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was isolated and purified through thin-layer silica gel chromatography (hexane/ethyl acetate=7/3) to obtain 25.2 mg of the entitled compound as a colorless oil.

1. customThe reaction liquid
2. washwashed with water and saturated saline water
3. dry with materialdried with anhydrous sodium sulfate
4. customThe solvent was evaporated away
5. dissolutionthe resulting residue was dissolved in dimethylformamide (2 mL)
6. additionmethyl iodide (0.080 mL) and potassium carbonate (198 mg) were added
7. stirringstirred at room temperature for 1 hour
8. customThe reaction liquid
9. washwashed with water and saturated saline water
10. dry with materialdried with anhydrous sodium sulfate
11. customThe solvent was evaporated away
12. customthe resulting residue was isolated
13. custompurified through thin-layer silica gel chromatography (hexane/ethyl acetate=7/3)