反应详情

温度

100 °C

An oven dried vial was charged with 1-(3,6-dibromo-9H-carbazol-9-yl)-2-methyl-3-phenoxypropan-2-ol (79.5 mg, 0.16 mmol), copper iodide (16 mg, 0.08 mmol), sodium cyanide (22 mg, 0.45 mmol) and potassium iodide (16 mg, 0.10 mmol). The sealed vial was nitrogen filled and evacuated three times before addition of N, N-dimethyl-1,2-ethanediamine (22.5 μl, 0.21 mmol) and anhydrous toluene (75 μl). The reaction was heated at 100° C. over 60 hours. The cooled mixture was diluted with EtOac, washed with water and brine. The organic layer was dried over Na2SO4, filtered and condensed. The crude mixture was purified on silica gel in 40% THF/hexanes. Yield=34%.

1. customAn oven dried vial
2. additionfilled
3. customevacuated three times
4. additionThe cooled mixture was diluted with EtOac
5. washwashed with water and brine
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. customcondensed
9. customThe crude mixture was purified on silica gel in 40% THF/hexanes