反应详情

A solution of 0.65 g (1.27 mmol) of [3-methyl-5-(3-trifluoromethyl-phenyl)-6-trimethylsilanylethynyl-pyridin-2-yl]-(4-pyrrolidin-1-yl-piperidin-1-yl)-methanone (intermediate 12) in 12 ml of EtOH/THF (5:1) was treated at RT with 0.35 g (2.53 mmol) of potassium carbonate. After 4 hours, the reaction mixture was poured into crashed ice, the pH was adjusted to 3-4 with hydrochloric acid (2 molar) 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/MeOH 1:0 to 9:1) to give 0.439 g (79%) of the title compound as brown solid. MS: 442.3 (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/MeOH 1:0 to 9:1)