反应详情

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of [5-(4-nitro-pyrazol-1-ylmethyl)-isoxazol-3-yl]-methanol (1.82 g, 8.20 mmol) in CH2Cl2 (25.0 mL) was added to an ice-chilled suspension of pyridinium chlorochromate (5.35 g, 24.36 mmol) in CH2Cl2 (25.0 mL). The reaction mixture was stirred for 4.5 h at rt. It was filtered over celite and the solvent was removed under reduced pressure. Purification of the residue by FC (50:50 hept-EA) gave the title compound as a colorless oil. TLC: rf (50:50 hept-EA)=0.36. LC-MS-conditions 02: tR=0.60 min.

1. temperaturechilled
2. filtrationIt was filtered over celite
3. customthe solvent was removed under reduced pressure
4. customPurification of the residue by FC (50:50 hept-EA)