反应详情

To a solution of 2.78 g (7.2 mmol) of 4-((S)-2-benzoyloxymethyl-pyrrolidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester in 80 ml of CH2Cl2 was added 5.83 ml of TFA (90% in water) drop by drop. After 16 hours, the reaction mixture was poured into crashed ice; then, the pH was adjusted to 9-10 with sodium carbonate solution and the mixture was extracted three times with CH2Cl2; the organic phases were washed with water, dried over magnesium sulfate, filtered and evaporated. The residue was purified by flash column chromatography [CH2Cl2 (sat. with NH3)/MeOH 1:0 to 9:1] to give 1.96 g (95%) of the title compound as yellow oil. MS: 289.1 (MH+).

1. additionthe reaction mixture was poured
2. extractionthe mixture was extracted three times with CH2Cl2
3. washthe organic phases were washed with water
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by flash column chromatography [CH2Cl2 (sat. with NH3)/MeOH 1:0 to 9:1]