反应详情

Compound 14c (17.3 g) was dissolved in tetrahydrofuran (180 ml) and methanol (180 ml), and iron powder (19.1 g) was added thereto. An ammonium chloride aqueous solution (1.67 mol/l, 110 ml) was added to the reaction mixture while refluxing under heating. The obtained mixture was refluxed under heating for 1 hour. After the mixture was allowed to cool, the iron powder was removed by Cerite filtration. Ethyl acetate and purified water were added to the filtrate, and extraction and washing were carried out. The organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was recrystallized with n-heptane to obtain Compound 14d (13.0 g, 85%) as an opalescent solid.

1. temperaturewhile refluxing
2. temperatureunder heating
3. temperatureThe obtained mixture was refluxed
4. temperatureunder heating for 1 hour
5. temperatureto cool
6. customthe iron powder was removed by Cerite filtration
7. customEthyl acetate and purified water
8. additionwere added to the filtrate, and extraction
9. washwashing
10. dry with materialThe organic layer was dried over anhydrous sodium sulfate
11. distillationthe solvent was distilled off under reduced pressure
12. customThe obtained residue was recrystallized with n-heptane