反应详情

3 g of the product of step (iii) (9.51 mmol) are dissolved in 60 ml of ethanol and 4.0 ml of 96% sulphuric acid are added, and the mixture is refluxed for 22 hours. The solvent is partially evaporated off and the remaining mixture is taken up with a mixture of 300 ml of a saturated sodium bicarbonate solution and 150 ml of ethyl acetate. The organic phase is washed with a saturated aqueous NaCl solution. The organic phase is dried and, after filtration, the solvent is evaporated off under reduced pressure. The crude product is purified by chromatography on a silica gel column, eluting with an 8/2 hexane-ethyl acetate mixture. The compound of the title is obtained in the form of a solid.

1. temperaturethe mixture is refluxed for 22 hours
2. customThe solvent is partially evaporated off
3. additionthe remaining mixture is taken up with a mixture of 300 ml of a saturated sodium bicarbonate solution and 150 ml of ethyl acetate
4. washThe organic phase is washed with a saturated aqueous NaCl solution
5. customThe organic phase is dried
6. filtrationafter filtration
7. customthe solvent is evaporated off under reduced pressure
8. customThe crude product is purified by chromatography on a silica gel column
9. washeluting with an 8/2 hexane-ethyl acetate mixture
10. customThe compound of the title is obtained in the form of a solid