反应详情

To a solution of 1.48 g (2.7 mmol) of [6-(4-methoxy-benzylamino)-3-methyl-5-(3-trifluoromethyl-phenyl)-pyridin-2-yl]-(4-pyrrolidin-1-yl-piperidin-1-yl)-methanone (example 6) in 75 ml of CH2Cl2 was added 12.2 ml=18.2 g (160 mmol) of trifluoroacetic acid and the reaction mixture was subsequently heated up to reflux. After two hours, it was poured into crashed ice, the pH was adjusted to 8-9 with sodium carbonate solution and it was extracted twice 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/MeOH 98:2 to 3:1) to give 1.04 g (90%) of the title compound as light yellow foam. MS: 433.3 (MH+).

1. temperaturethe reaction mixture was subsequently heated up
2. temperatureto reflux
3. additionit was poured
4. extractionwas extracted twice with CH2Cl2
5. washthe organic phases were washed with water
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customevaporated
9. customThe residue was purified by flash column chromatography (CH2Cl2/MeOH 98:2 to 3:1)