反应详情

温度

75 °C

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 1-[2-(3-nitro-pyrazol-1-ylmethyl)-oxazol-4-yl]-ethanone (48 mg, 0.20 mmol), iron powder (34 mg, 0.61 mmol) and NH4Cl (56 mg, 1.03 mmol) in a mixture of EtOH (2.0 mL) and water (1.0 mL) was stirred at 75° C. for 60 min. The reaction mixture was filtered while hot and concentrated under reduced pressure. CH2Cl2 (10 mL) was added followed by water (10 mL). The aq. layer was extracted with CH2Cl2 (2×10 mL) and the combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a yellow oil. TLC: rf (EA)=0.13. LC-MS-conditions 02: tR=0.38 min; [M+H]+=207.40.

1. filtrationThe reaction mixture was filtered while hot and
2. concentrationconcentrated under reduced pressure
3. additionCH2Cl2 (10 mL) was added
4. extractionThe aq. layer was extracted with CH2Cl2 (2×10 mL)
5. dry with materialextracts were dried over Na2SO4
6. filtrationfiltered
7. customthe solvents were removed under reduced pressure