反应详情

To a dimethylformamide solution (600 μL) of 2-(3,4-dichlorophenyl)-3-hydroxy-4-methylcarbonylthiophene (30 mg, 0.10 mmol) and methyl 1-hydrazinothiocarbonyl-piperidine-4-carboxylate (46 mg, 0.20 mmol) prepared in Reference Synthetic Example 2, concentrated hydrochloric acid (9 μL, 0.1 mmol) was added at room temperature, and the resulting solution was stirred at room temperature for 8 hours, then mixed with water and extracted with ethyl acetate. The extract was washed with 1 M hydrochloric acid and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/1) and recrystallized from chloroform to give the desired product (yield 55%).

1. additionwas added at room temperature
2. extractionextracted with ethyl acetate
3. washThe extract was washed with 1 M hydrochloric acid and saturated aqueous sodium chloride
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customThe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/1)
7. customrecrystallized from chloroform