反应详情

温度

0 °C

1-tert-Butyl 2-methyl 2-{2-[(2-chlorophenyl)amino]ethyl}pyrrolidine-1,2-dicarboxylate, was dissolved in anhydrous THF (4 mL) and cooled to 0° C. To this cooled solution was added isopropylmagnesium chloride in THF (2.0 M, 2 mL). The reaction vial was then sealed and heated to 64° C. and stirred for 18 h. The reaction mixture was then diluted with EtOAc and quenched by the addition of water. The crude mixture was filtered through a pad of diatomaceous earth and the filter pad was washed several times with EtOAc. The organic and aqueous layers of the filtrate were separated. The aqueous phase was extracted with EtOAc (3×10 mL) and the combined organic phases were washed with brine (2×5 mL), then dried (NaSO4), filtered, and concentrated in vacuo to afford the desired product. LC-MS: 251.1 (M−Boc+2H)+ and 295.1 (M−t-Bu+2H)+.

1. customThe reaction vial was then sealed
2. temperatureheated to 64° C.
3. customquenched by the addition of water
4. filtrationThe crude mixture was filtered through a pad of diatomaceous earth
5. washthe filter pad was washed several times with EtOAc
6. customThe organic and aqueous layers of the filtrate were separated
7. extractionThe aqueous phase was extracted with EtOAc (3×10 mL)
8. washthe combined organic phases were washed with brine (2×5 mL)
9. dry with materialdried (NaSO4)
10. filtrationfiltered
11. concentrationconcentrated in vacuo