反应详情

温度

70 °C

To a solution of 1 (0.1 g, 0.35 mmol) in acetic acid was added sodium acetate (29 mg, 0.35 mmol) and palladium on charcoal (20 mg). The suspension was heated up to 70° C. under hydrogen at 3.5 bar for 3 h. After cooling to rt., the suspension was filtered through celite and the acetic acid evaporated. The bright yellow powder was taken up in ethyl acetate and aqueous sodium hydroxide 10%. After 3 extractions the organic phases were thoroughly washed with brine then dried over MgSO4 and concentrated to dryness. After purification by preparative HPLC and drying under vacuum at 50° C., 12 mg (13%) of the title compound were obtained as a yellow powder.

1. temperatureAfter cooling to rt
2. filtration, the suspension was filtered through celite
3. customthe acetic acid evaporated
4. extractionAfter 3 extractions the organic phases
5. washwere thoroughly washed with brine
6. dry with materialthen dried over MgSO4
7. concentrationconcentrated to dryness
8. customAfter purification by preparative HPLC
9. customdrying under vacuum at 50° C.