反应详情

To a solution of the title compound from Example 71 Step A (0.50 g, 2.17 mmol) in N,N-dimethylformamide (6.8 mL) and tetrahydrofuran (6.8 mL) was added sodium hydride (60% dispersion in mineral oil, 0.435 g, 10.9 mmol). After stirring for 15 minutes, 1,2-dibromoethane (0.56 ml, 6.5 mmol) was added. After stirring overnight, the reaction was poured into water and extracted with ethyl acetate. The combined organic extracts were washed with water and saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and concentrated. Purification by flash chromatography on silica gel (20-80% ethyl acetate in hexanes) provided the title compound: LCMS m/z 257.78 [M+2+H]+; 1H NMR (500 MHz, CD3OD) δ 8.53 (s, 1H), 8.49 (s, 1H), 8.02 (s, 1H), 3.63 (s, 3H), 1.64 (m, 2H), 1.29 (m, 2H).

1. stirringAfter stirring overnight
2. extractionextracted with ethyl acetate
3. washThe combined organic extracts were washed with water and saturated aqueous sodium chloride solution
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by flash chromatography on silica gel (20-80% ethyl acetate in hexanes)