反应详情

温度

-40 °C

6-Nitroindole-1H-indole (35.6 g, 220 mmol) was dissolved in 750 mL of DMF and NaH (50%, 12 g, 250 mmol) was added in portions and the mixture was stirred for 1 hour. The mixture was cooled to −40° C. and the solution of the mesylate was added dropwise. The mixture was allowed to reach room temperature overnight. The mixture was quenched with water and extracted with ethyl acetate (2×). The combined organic layers were washed with water (2×) and brine and dried over Na2SO4. After concentration in vacuo the material was purified by means of column chromatography (silica, heptane/ethyl acetate (1:1)→(1:4)) affording compound the title compound as a yellow solid (14 g, 55 mmol, 39%).

1. waitto reach room temperature overnight
2. customThe mixture was quenched with water
3. extractionextracted with ethyl acetate (2×)
4. washThe combined organic layers were washed with water (2×) and brine
5. dry with materialdried over Na2SO4
6. concentrationAfter concentration in vacuo the material
7. customwas purified by means of column chromatography (silica, heptane/ethyl acetate (1:1)→(1:4))