反应详情

A solution of 1-{4-chloro-6-[1-(1-ethoxyethyl)-1H-pyrazol-4-yl]-3′,5′-difluorobiphenyl-2-yl}ethanone (190 mg, 0.47 mmol), ammonium acetate (360 mg, 4.7 mmol) in methanol (2 mL) and acetonitrile (2 mL) was heated at 65° C. for 3 hours. The reaction mixture was quenched with acetic acid (˜100 uL) and poured into sodium bicarbonate (50 mL). This mixture was extracted with dichloromethane (3×60 mL) and the combined organic layers were washed with brine, dried with sodium sulfate, filtered, and concentrated to a crude residue. Purification via preparative LCMS (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.1% ammonium hydroxide, at flow rate of 60 mL/min) gave the desired product (60 mg, 32%). LCMS for C21H23ClF2N3O (M+H)+: m/z=406.1. Found: 406.1.

1. customThe reaction mixture was quenched with acetic acid (˜100 uL)
2. additionpoured into sodium bicarbonate (50 mL)
3. extractionThis mixture was extracted with dichloromethane (3×60 mL)
4. washthe combined organic layers were washed with brine
5. dry with materialdried with sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated to a crude residue
8. customPurification via preparative LCMS (XBridge C18 column
9. washeluting with a gradient of acetonitrile/water containing 0.1% ammonium hydroxide, at flow rate of 60 mL/min)