反应详情

温度

0 °C

To a solution of 5-methyl-3-(3-nitropyridin-4-yl)cyclohex-2-enone (1.0 equiv.) in EtOH (0.3 M) was added CeCl3-7H2O (1.2 equiv.). The reaction was cooled to 0° C., then NaBH4 (1.2 equiv.) was added in portions. Stirred for 1 h at 0° C., then quenched by adding water, concentrated to remove the EtOH, added EtOAc, extracted the organics, washed with brine, then dried with Na2SO4, filtered and concentrated to yield cis-(+/−)-5-methyl-3-(3-nitropyridin-4-yl)cyclohex-2-enol (94%). LC/MS=235.2 (M+H), LC=2.62 min.

1. customquenched
2. additionby adding water
3. concentrationconcentrated
4. customto remove the EtOH
5. additionadded EtOAc
6. extractionextracted the organics,
7. washwashed with brine
8. dry with materialdried with Na2SO4
9. filtrationfiltered
10. concentrationconcentrated