反应详情

Into a 1 l capacity three-necked flask were added the compound obtained in the above item (ii) (36.2 g, 0.15 mol), 2N-hydrochloric acid (142 ml) and tetrahydrofuran (560 ml), followed by refluxing these for one hour, distilling off tetrahydrofuran, adding water (100 ml) to extract with ethyl acetate, washing the extract with 1N-NaOH aqueous solution, washing with water till the washing water became neutral, drying over magnesium sulfate, removing magnesium sulfate, concentrating under reduced pressure, recrystallizing from a mixed solvent of heptane with ethyl acetate and drying to obtain white crystals (20.5 g). The NMR spectra of this product accorded with those of the captioned compound.

1. additionInto a 1 l capacity three-necked flask were added the compound
2. temperatureby refluxing these for one hour
3. distillationdistilling off tetrahydrofuran
4. additionadding water (100 ml)
5. extractionto extract with ethyl acetate
6. washwashing the
7. extractionextract with 1N-NaOH aqueous solution
8. washwashing with water till the washing water
9. dry with materialdrying over magnesium sulfate
10. customremoving magnesium sulfate
11. concentrationconcentrating under reduced pressure
12. customrecrystallizing from a mixed solvent of heptane with ethyl acetate
13. customdrying