反应详情

And, then, the 2-(2-fluoro-4-nitrophenyl)-octahydro-5-hydroxycyclopenta[c]pyrrol (44.4 mmol) prepared in the step 2 was dissolved in 100 ml of methylene chloride and slowly added over 30 minutes, the mixture was stirred for 1 hour while maintaining the temperature, and then, 30.93 ml (221.9 mmol) of triethylamine was slowly added over 20 minutes, the temperature was raised to room temperature, and the mixture was stirred for 2 hours. After the reaction was completed, 100 mL of methylene chloride was added to dilute the mixture, and then, the mixture was washed with water and a saturated aqueous solution of sodium chloride, and the organic layer was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The concentrate was recrystallized under ethanol solvent to obtain 11.1 g (95%) of the title compound.

1. additionslowly added over 30 minutes
2. temperaturewhile maintaining the temperature
3. stirringthe mixture was stirred for 2 hours
4. additionto dilute the mixture
5. washthe mixture was washed with water
6. dry with materiala saturated aqueous solution of sodium chloride, and the organic layer was dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe concentrate was recrystallized under ethanol solvent