反应详情

To a suspension of 13-bromo-12-fluoro-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (2.00 g, 4.93 mmol) and LiCl (620 mg, 14.8 mmol) in dry THF (15 mL), was added tri-n-butyl(1-ethoxyvinyl)tin (1.78 g, 4.93 mmol) and tetrakis(triphenylphosphine) palladium (185 mg, 0.160 mmol) under nitrogen at room temperature. The resultant mixture was heated under 80° C. for 24 h in a seal tube. After cooling down, the mixture was diluted with THF, treated with an aqueous 0.16 M potassium fluoride solution (20 ml), and stirred at ambient temperature for 1 h. The precipitated tri-nbutylstannyl fluoride was removed by filtration. The filtrate was evaporated under reduced pressure to give an aqueous suspension, which was extracted with ethyl acetate. The combined organic layers were washed with water and evaporated in vacuo to give the crude product (1.97 g, over 100% yield) a yellow solid, which was used directly in the next step without further purification. LCMS m/z [M+H]+ 398.1

1. temperatureAfter cooling down
2. customThe precipitated tri-nbutylstannyl fluoride was removed by filtration
3. customThe filtrate was evaporated under reduced pressure
4. customto give an aqueous suspension, which
5. extractionwas extracted with ethyl acetate
6. washThe combined organic layers were washed with water
7. customevaporated in vacuo