反应详情

To a degassed solution of 0.20 g (0.44 mmol) of [6-chloro-3-methyl-5-(3-trifluoromethyl-phenyl)-pyridin-2-yl]-(4-pyrrolidin-1-yl-piperidin-1-yl)-methanone (example 3) in 8.0 ml of DMF was added 0.051 g (0.044 mmol) of tetrakis-(triphenylphosphine)-palladium and the reaction mixture was stirred for 20 min at RT. Then, 0.49 g (1.32 mmol) of 2-tributylstannanyl-pyrazine were added and the reaction was heated up to 100° C. After 6 hours, it was cooled down to RT, poured into crashed ice and extracted three times with EtOAc; 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 0.11 g (50%) of the title compound as yellow oil. MS: 496.2 (MH−).

1. temperaturethe reaction was heated up to 100° C
2. waitAfter 6 hours
3. temperatureit was cooled down to RT
4. additionpoured
5. extractionextracted three times with EtOAc
6. washthe organic phases were washed with water
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified by flash column chromatography (CH2Cl2/MeOH 1:0 to 9:1)