反应详情

温度

0 °C

6-(Methoxycarbonyl)-3-methyl-1H-indazole (0.40 g, 2.1 mmol) was dissolved in dimethylformamide (15 ml) and the mixture was ice-cooled. Sodium hydride (85 mg, 60% suspension in oil, 2.1 mmol as NaH) was added and the mixture was stirred at 0° C. for 30 min. 2,4-Dichlorobenzyl chloride (0.45 g, 2.31 mmol) was added and the mixture was stirred at room temperature for 18 hr. The reaction mixture was extracted with ethyl acetate/water. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The drying agent was filtered off and the filtrate was concentrated under reduced pressure. The obtained crystalline residue was separated and purified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1) to give the objective compound (0.54 g, 74%) as colorless crystals.

1. temperaturecooled
2. stirringthe mixture was stirred at room temperature for 18 hr
3. extractionThe reaction mixture was extracted with ethyl acetate/water
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationThe drying agent was filtered off
7. concentrationthe filtrate was concentrated under reduced pressure
8. customThe obtained crystalline residue was separated
9. custompurified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1)