反应详情

温度

180 °C

4-Bromo-3-fluorophenol (0.5 g, 2.61 mmol) was added to a solution of sodium hydride (0.115 g, 2.90 mmol) in DMF (5 ml). After stiffing for 10 minutes 4-nitro-2-picoline N-oxide (0.37 g, 2.41 mmol) was added. The reaction mixture was heated at 180° C. for 1 hour under microwave irradiation. After cooling to room temperature the mixture was filtered through diatomaceous earth and this was thoroughly washed with EtOAc. The filtrate was washed with water (2×25 ml), the organic fraction was dried (Na2SO4) and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; 0-3% methanol/DCM as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate D12 (0.33 g, 49%).

1. temperatureAfter cooling to room temperature the mixture
2. filtrationwas filtered through diatomaceous earth
3. washthis was thoroughly washed with EtOAc
4. washThe filtrate was washed with water (2×25 ml)
5. dry with materialthe organic fraction was dried (Na2SO4)
6. customthe solvent evaporated in vacuo
7. customThe crude product was purified by column chromatography (silica gel; 0-3% methanol/DCM as eluent)
8. customThe desired fractions were collected
9. customevaporated in vacuo
10. customto yield intermediate D12 (0.33 g, 49%)