反应详情

To a mixture of 2-methylbenzophenone (2.0 g, 10.2 mmol) and N-boc-3-pyrrolidone (1.89 g, 10.2 mmol) in THF was added zinc powder (3.3 g, 59 mmol) at 10-15° C. and stirred for 15 min. To the reaction mixture was added TiCl4 (4.76 g, 25 mmol) and the contents were brought to 60° C. and stirred for 8 h. The reaction mixture was allowed to cool to room temperature, diluted HCl was added and extracted with EtOAc. The organic layer was washed with aqueous sodium potassium tartarate solution. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford the crude product which was washed with n-hexane to afford 1.8 g of (Z)-3-(phenyl(m-tolyl)methylene)pyrrolidine.

1. customwere brought to 60° C.
2. stirringstirred for 8 h
3. extractionextracted with EtOAc
4. washThe organic layer was washed with aqueous sodium potassium tartarate solution
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customto afford the crude product which
8. washwas washed with n-hexane