反应详情

The octahydro-5-hydroxycyclopenta[c]pyrrol hydrochloride (44.4 mmol) prepared in the step 1 was dissolved in 100 ml of acetonitrile, and 4.91 ml (44.4 mmol) of 1,2-difluoro-4-nitrobenzene and 23.20 ml (133.2 mmol) of N,N-diisopropylethylamine were added, and the mixture was heat to reflux for 6 hours. After the reaction was completed, the temperature was lowered to room temperature, and the mixture was concentrated under reduced pressure to remove the solvent. The solvent-free concentrate was dissolved in ethyl acetate, and washed with distilled water, and then, the organic layer was dried over magnesium sulfate, filtered and concentrated under reduced pressure to obtain the title compound, of which NMR data is as follow.

1. temperaturethe mixture was heat
2. temperatureto reflux for 6 hours
3. customwas lowered to room temperature
4. concentrationthe mixture was concentrated under reduced pressure
5. customto remove the solvent
6. concentrationThe solvent-free concentrate
7. dissolutionwas dissolved in ethyl acetate
8. washwashed with distilled water
9. dry with materialthe organic layer was dried over magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated under reduced pressure