反应详情

To a solution of 0.75 mmol 3-(4-trifluoromethyl-phenoxy)-pyrrolidine-1-carboxylic acid tert-butyl ester in 20 ml dioxane at 0° C. was added dropwise 9.20 mmol trifluoroacetic acid, and the reaction mixture was then stirred at RT for 3 h. The reaction mixture was then concentrated in vacuo, and the residue resuspended in ethyl acetate and washed with 1 M aqueous hydrochloric acid. The aqueous phase was separated and then made basic by addition of 1 M aqueous sodium hydroxide solution and subsequently extracted with ethyl acetate. The organic phase was dried over sodium sulfate and concentrated in vacuo to afford the title compound as a white amorphous solid (yield 69%). MS (m/e): 232.1 (M+H+, 100%).

1. concentrationThe reaction mixture was then concentrated in vacuo
2. washwashed with 1 M aqueous hydrochloric acid
3. customThe aqueous phase was separated
4. additionmade basic by addition of 1 M aqueous sodium hydroxide solution
5. extractionsubsequently extracted with ethyl acetate
6. dry with materialThe organic phase was dried over sodium sulfate
7. concentrationconcentrated in vacuo