反应详情

温度

60 °C

To 3-bromo-4-fluoronitrobenzene (7.05 g, 32.0 mmol) and ethanethiol (2.6 mL, 35.2 mmol) in DMF (20 mL) was added potassium carbonate (4.87 g, 35.2 mmol). The reaction mixture was heated to 60° C. overnight. After cooling, the mixture was filtered over celite and washed with ethyl acetate. The combined filtrate and washings were concentrated. The residue was redissolved in ethyl acetate and washed with water (3×) and then dried over sodium sulfate. The filtrate was concentrated and purified by flash column chromatography to give 100A (8.09 g, 96% yield) as a solid. 1H NMR (400 MHz, Methanol-d4) δ ppm 1.41 (t, J=7.34 Hz, 3H) 3.11 (q, J=7.42 Hz, 2H) 7.45 (d, J=9.05 Hz, 8H) 8.17 (dd, J=8.80, 2.45 Hz, 7H) 8.37 (d, J=2.45 Hz, 7H).

1. temperatureAfter cooling
2. filtrationthe mixture was filtered over celite
3. washwashed with ethyl acetate
4. concentrationThe combined filtrate and washings were concentrated
5. dissolutionThe residue was redissolved in ethyl acetate
6. washwashed with water (3×)
7. dry with materialdried over sodium sulfate
8. concentrationThe filtrate was concentrated
9. custompurified by flash column chromatography