反应详情

温度

100 °C

A solution of 1-[2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]methanamine (Intermediate 5, 300 mg, 1.394 mmol) in dry N,N-dimethylformamide (DMF) (15.000 mL) was treated with 4-chloro-6-(fluoromethyl)-5-methylpyrimidine (Intermediate 51, 336 mg, 2.091 mmol) and triethylamine (0.389 mL, 2.79 mmol). The reaction mixture was heated at 100° C. and stirred for 28 hours. The reaction mixture was poured into water (20 mL) and extracted with ethyl acetate (2×20 mL). The organic extract was then dried under magnesium sulphate, filtered and the solvent removed under reduced pressure. The residue was purified on SP4 column chromatography (25+M) eluting with 0-100% isohexane-ethyl acetate. Product containing fractions were combined and evaporated under reduced pressure. The white residue was then dissolved in 1:1 ethyl acetate:methanol (2 mL) and 1M HCl in diethylether (0.05 mL, 0.543 mmol) was added. The mixture was then evaporated to dryness to give the title compound as a white solid (15 mg);

1. extractionextracted with ethyl acetate (2×20 mL)
2. extractionThe organic extract
3. customwas then dried under magnesium sulphate
4. filtrationfiltered
5. customthe solvent removed under reduced pressure
6. customThe residue was purified on SP4 column chromatography (25+M)
7. washeluting with 0-100% isohexane-ethyl acetate
8. additionProduct containing fractions
9. customevaporated under reduced pressure
10. dissolutionThe white residue was then dissolved in 1:1 ethyl acetate
11. customThe mixture was then evaporated to dryness