反应详情

温度

70 °C

0.7 g of the product of Step 1 was added into 80 ml of ethanol:water (v/v=31), then 1.0 g iron powder and 0.4 g ammonium chloride. After addition, the reaction mixture was heated to 70° C. and reacted for 30 min. The completion of reaction was indicated by TLC. The reaction mixture was filtered, and the filter cake was washed with hot ethanol repeatedly. Then the filtrate was concentrated under reduced pressure to give a white solid. Then 20 ml potassium carbonate solution (10%) was added into the solid. The mixture was stirred, left to stand, filtered, and dried to give a light yellow solid (0.7 g).

1. additionAfter addition
2. customreacted for 30 min
3. customThe completion of reaction
4. filtrationThe reaction mixture was filtered
5. washthe filter cake was washed with hot ethanol repeatedly
6. concentrationThen the filtrate was concentrated under reduced pressure
7. customto give a white solid
8. waitleft
9. filtrationfiltered
10. customdried