反应详情

54.1 g (390 mmol) M24 obtained from the preceding reaction step was dissolved in 380 ml absolute ethanol and 9 ml conc. H2SO4 was added. The mixture was heated at reflux for 18 hours. Most of the ethanol was evaporated and the residue was dissolved in 400 ml CHCl3/100 ml water and basified with powder NaHCO3. The organic phase was washed with 2×400 ml saturated NaHCO3 and dried over Na2SO4. The solvent was evaporated to afford 58.3 g clear oil (yield: 89%).

1. temperatureThe mixture was heated
2. temperatureat reflux for 18 hours
3. customMost of the ethanol was evaporated
4. dissolutionthe residue was dissolved in 400 ml CHCl3/100 ml water and basified with powder NaHCO3
5. washThe organic phase was washed with 2×400 ml saturated NaHCO3
6. dry with materialdried over Na2SO4
7. customThe solvent was evaporated