反应详情

温度

75 °C

A suspension of Example 1D (1.01 g, 3.53 mmol) in ethanol (60 mL), THF (20 mL), and water (10 mL) was treated with NH4Cl (0.19 g, 3.53 mmol) and iron powder (1.18 g, 21.2 mmol), and stirred at 70-80° C. for 1 hour. The mixture was diluted with ethanol (40 mL) and filtered through a pad of diatomaceous earth (Celite®) while still hot. The pad was washed with ethanol and the filtrate was concentrated. The concentrate was diluted with water and extracted three times with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated to provide 1 g of the desired product. MS (CI) m/e 257 (M+H)+; 1H NMR (300 MHz, DMSO-d6) δ 8.23 (s, 1H); 7.01 (d, J=8.4 Hz, 2H); 6.70 (d, J=8.4 Hz, 2H); 5.39 (s, 2H); 2.27 (s, 3H); Anal. Calcd. for C13H12N4S.0.2C4H8O2.0.2H2O: C, 59.72; H, 5.08; N, 20.19. Found: 59.64; H, 4.99; N, 20.22.

1. filtrationfiltered through a pad of diatomaceous earth (Celite®) while still hot
2. washThe pad was washed with ethanol
3. concentrationthe filtrate was concentrated
4. additionThe concentrate was diluted with water
5. extractionextracted three times with ethyl acetate
6. washThe combined extracts were washed with brine
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated