反应详情

A solution of tert-butyl[4-[[2-[3-(3-fluorophenyl)propanoyl]hydrazino]carbonyl]-2-pyridyl]carbamate (1.00 g, 2.48 mmol), p-toluenesulfonyl chloride (946 mg, 4.96 mmol) and triethylamine (1.72 mL, 12.4 mmol) in tetrahydrofuran (30 mL) was heated under reflux for 17 hr. After cooling, the reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=95/5-0/100), and recrystallized from ethyl acetate to give the title compound (0.70 g, yield 73%) as colorless crystals.

1. temperatureunder reflux for 17 hr
2. temperatureAfter cooling
3. washwashed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=95/5-0/100)
7. customrecrystallized from ethyl acetate