反应详情

1-Benzyl-3-(3,5-dichloro-4-fluorophenyl)-3-(trifluoromethyl)pyrrolidine (3.7 g) was dissolved in 1,2-dichloroethane (20 ml), added with 1-chloroethyl chloroformate (2.7 g) at room temperature, and then refluxed under heating for 3 hours. The reaction solution was concentrated under reduced pressure, and the residue obtained was added with methanol (30 ml) and further refluxed under heating for 2 hours. The reaction solution was concentrated under reduced pressure and the residue obtained was added with t-butyl methyl ether and water to separate the aqueous layer. After that, the organic layer was again washed with a 1 M aqueous solution of hydrochloric acid, and the aqueous layers were combined, added with a saturated aqueous solution of potassium carbonate to make the liquid alkaline, and extracted with t-butyl methyl ether. The aqueous phase was extracted again with t-butyl methyl ether, and the organic layers were combined, dried over magnesium sulfate, filtered and concentrated under reduced pressure to obtain 3-(3,5-dichloro-4-fluorophenyl)-3-(trifluoromethyl)pyrrolidine (2.6 g).

1. temperaturerefluxed
2. temperatureunder heating for 3 hours
3. concentrationThe reaction solution was concentrated under reduced pressure
4. customthe residue obtained
5. temperaturefurther refluxed
6. temperatureunder heating for 2 hours
7. concentrationThe reaction solution was concentrated under reduced pressure
8. customthe residue obtained
9. customto separate the aqueous layer
10. washAfter that, the organic layer was again washed with a 1 M aqueous solution of hydrochloric acid
11. additionadded with a saturated aqueous solution of potassium carbonate
12. extractionextracted with t-butyl methyl ether
13. extractionThe aqueous phase was extracted again with t-butyl methyl ether
14. dry with materialdried over magnesium sulfate
15. filtrationfiltered
16. concentrationconcentrated under reduced pressure