反应详情

温度

-40 °C

Into a 3-L 4-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen was placed tetrahydrofuran (1200 mL), 9-bromo-3,4-diiodo-2,5-diazatetracyclo[11.1.1.0[2,6].0[7,12]]pentadeca-3,5,7,9,11-pentaene (119.3 g, 226.40 mmol, 1.00 equiv), followed by the addition of EtMgBr (90.7 mL, 1.20 equiv) dropwise with stirring at −40° C. The resulting solution was stirred at −40° C. for 1 h. This reaction was repeated for 2 more times. The reaction was then quenched by the addition of 500 mL of 5% hydrogen chloride and extracted with 3×500 mL of dichloromethane. The organic layers were combined, dried over anhydrous sodium sulfate and concentrated under vacuum to afford 259 g (97%) of 9-bromo-4-iodo-2,5-diazatetracyclo[11.1.1.0[2,6].0[7,12]]pentadeca-3,5,7,9,11-pentaene as a brown solid.

1. customInto a 3-L 4-necked round-bottom flask purged
2. temperaturemaintained with an inert atmosphere of nitrogen
3. stirringThe resulting solution was stirred at −40° C. for 1 h
4. customThe reaction was then quenched by the addition of 500 mL of 5% hydrogen chloride
5. extractionextracted with 3×500 mL of dichloromethane
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under vacuum