反应详情

20 g of molecular sieve 3 Å are added to 15 g (50 mmol) of the compound from Example 2 and 20 g (164 mmol) of N-aminopyrrolidine hydrochloride in 150 ml of toluene AR and the mixture is heated to reflux for 48 hours. The mixture is cooled, filtered and washed well with toluene. The toluene solutions are combined and extracted 3×using 1N hydrochloric acid. The organic phase is subsequently washed using saturated sodium hydrogen carbonate solution, dried over magnesium sulphate and concentrated in vacuo. The residue is stirred with a little ethanol, cooled and filtered off with suction. After drying in a desiccator, 2.3 g of substance are obtained.

1. temperaturethe mixture is heated
2. temperatureto reflux for 48 hours
3. temperatureThe mixture is cooled
4. filtrationfiltered
5. washwashed well with toluene
6. extractionextracted 3×
7. washThe organic phase is subsequently washed
8. dry with materialdried over magnesium sulphate
9. concentrationconcentrated in vacuo
10. temperaturecooled
11. filtrationfiltered off with suction
12. customAfter drying in a desiccator
13. custom2.3 g of substance are obtained