反应详情

To a solution of N-[6-chloro-4-(4-fluoro-2-methoxy-phenyl)-pyridazin-3-yl]-3-methanesulfonyl-N-methyl-5-trifluoromethyl-benzamide (50 mg, 96.5 μmol, example 1) in methanol (2 mL) and ethyl acetate (2 mL) was added palladium on activated charcoal (10%, 10 mg, 96.5 μmol) under argon atmosphere. The reaction apparatus was evacuated and purged with hydrogen gas. The reaction was stirred under a hydrogen atmosphere of 1.7 bar for 8 hours. The reaction mixture was filtered over dicalite and the filtrate was concentrated under vacuum. The residue was purified by silica gel chromatography on a 10 g column using an MPLC (Flashmaster) system eluting with a gradient of n-heptane:ethyl acetate (100:0 to 0:100). The product was purified by preparative HPLC (Gemini NX column) with a gradient of methanol:water with 0.05% formic acid (80:20 to 98:2) to give the title compound as a light brown solid (13 mg, 27.9%). MS (ESI+): m/z=484.095 ([M+H]+).

1. customThe reaction apparatus was evacuated
2. custompurged with hydrogen gas
3. filtrationThe reaction mixture was filtered over dicalite
4. concentrationthe filtrate was concentrated under vacuum
5. customThe residue was purified by silica gel chromatography on a 10 g column
6. washeluting with a gradient of n-heptane:ethyl acetate (100:0 to 0:100)
7. customThe product was purified by preparative HPLC (Gemini NX column) with a gradient of methanol