反应详情

1-[(2,4-Dichlorophenyl)methyl]-1H-pyrazol-3-amine (40 μl, 0.23 mmol, Art-Chem GmbH) was dissolved in dichloromethane (2 ml). Triethylamine (64 μl, 0.46 mmol) and then 2,6-difluorobenzoyl chloride (49 mg, 0.28 mmol, Aldrich) were added and the reaction was stirred at room temperature for 2 h. The reaction was quenched by addition of water (5 ml). The organic phase was separated (by hydrophobic frit) and concentrated under a flow of nitrogen. The residue was purified by MDAP (supelcosil ABZ+Plus column) eluting with solvents A/B (A: Water+0.1% Formic acid, B: MeCN:Water 95:5+0.05% Formic acid) (Method A). The appropriate fractions were concentrated in vacuo then under nitrogen flow. The sample was dissolved in methanol and applied to a 5 g aminopropyl ion exchange cartridge (prewashed with MeOH) and eluted with MeOH. The relevant fractions were combined and concentrated to give the title compound as a colourless solid (36 mg); LCMS: (System 1) MH+=382/384, tRET=3.47 min.

1. customThe reaction was quenched by addition of water (5 ml)
2. customThe organic phase was separated (by hydrophobic frit)
3. concentrationconcentrated under a flow of nitrogen
4. customThe residue was purified by MDAP (supelcosil ABZ+Plus column)
5. washeluting with solvents A/B (A: Water+0.1% Formic acid, B
6. concentrationThe appropriate fractions were concentrated in vacuo
7. dissolutionThe sample was dissolved in methanol
8. washeluted with MeOH
9. concentrationconcentrated