反应详情

27 mg (0.31 mmol) of (ethyl)dimethylsilane and 15 mg (0.03 mmol) of bis(tri-tert-butylphosphine)palladium are added to a suspension of 0.15 g (0.28 mmol) of N-[6-(azetidin-1-yl)pyridin-3-yl]-5-iodo-1-[(3-fluorophenyl)methyl]-1H-indole-2-carboxamide, prepared according to the protocol described in stage 8.3, and of 0.18 g (0.85 mmol) of potassium triphosphate in 2 ml of dry 1-methyl-2-pyrrolidinone (NMP), maintained under an inert atmosphere. The reaction mixture is then stirred at ambient temperature under an inert atmosphere for 6 h and then diluted with 40 ml of a mixture of water and ethyl acetate (1/1). The resulting mixture is separated by settling out and the aqueous phase is extracted with 2×10 ml of ethyl acetate. The combined organic phases are dried over sodium sulphate, filtered and concentrated under reduced pressure. The resulting oil is purified by silica gel column chromatography, elution being carried out with a mixture of heptane and ethyl acetate. 108 mg of the expected product are isolated.

1. customprepared
2. customThe resulting mixture is separated
3. extractionthe aqueous phase is extracted with 2×10 ml of ethyl acetate
4. dry with materialThe combined organic phases are dried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe resulting oil is purified by silica gel column chromatography, elution
8. additionbeing carried out with a mixture of heptane and ethyl acetate