反应详情

温度

125 °C

0.90 g (1.99 mmol) of [6-chloro-3-methyl-5-(3-trifluoromethyl-phenyl)-pyridin-2-yl]-(4-pyrrolidin-1-yl-piperidin-1-yl)-methanone (example 3), 0.042 g (0.06 mmol) of bis(triphenylphosphine)palladium(II) chloride and 0.021 g (0.11 mmol) of copper(I) iodide were suspended in 2.0 ml of triethylamine. After addition of 2.14 ml=1.50 g (15.0 mmol) of ethinyltrimethylsilane, the reaction vessel was sealed, heated up to 125° C. and stirring continued for four days. The reaction mixture was then poured into crashed ice and 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 0.693 g (68%) of the title compound as dark brown oil. MS: 514.4 (MH+).

1. customthe reaction vessel was sealed
2. additionThe reaction mixture was then poured
3. extractionextracted three times with CH2Cl2
4. washthe organic phases were washed with water
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by flash column chromatography (CH2Cl2/MeOH 1:0 to 9:1)