反应详情

温度

0 °C

In a 100 mL round bottom flask, was added 70 mg 4-(3,4-Dichloro-phenyl)-5-pyridin-4-yl-1-pyridin-3-ylmethyl-pyrazolidin-3-one and 10 mL THF, stirred at 0° C. under nitrogen. 0.26 mL 1 M LHMDS in THF was added drop wise. After stirred at 0° C. for 30 min. 0.017 mL iodomethane was added drop wise. The resulted mixture was stirred from 0° C. to rt for 2 hour, quenched with 20 mL sat. NH4Cl, extracted with dichloromethane 3×25 mL. The crude MS showed the desired 4-(3,4-Dichloro-phenyl)-2-methyl-5-pyridin-4-yl-1-pyridin-3-ylmethyl-pyrazolidin-3-one was there, MS (ES+): 413 (M+H)+. The organic phase was dried over anhydrous Na2SO4. After purification by flash chromatography, the 4-(3,4-Dichloro-phenyl)-5-pyridin-4-yl-1-pyridin-3-ylmethyl-pyrazolidin-3-one was oxidized on column and obtained the 4-(3,4-Dichloro-phenyl)-2-methyl-5-pyridin-4-yl-1-pyridin-3-ylmethyl-1,2-dihydro-pyrazol-3-one 12 mg as light yellow solid. MS (ES+): 411 (M+H)+.

1. stirringAfter stirred at 0° C. for 30 min
2. stirringThe resulted mixture was stirred from 0° C. to rt for 2 hour
3. customquenched with 20 mL sat. NH4Cl
4. extractionextracted with dichloromethane 3×25 mL
5. dry with materialThe organic phase was dried over anhydrous Na2SO4
6. customAfter purification by flash chromatography