反应详情

温度

110 °C

9.4 g of the product from Example 5 and 19.2 g of iron turnings are warmed at 80° C. for 1 hour in 190 ml of acetic acid. The mixture is then heated briefly to 110° C. and filtered while hot. Ice-water is then added to the filtrate, and the precipitated solid is isolated. After drying at 110° C., the product is recrystallized from glycol monomethyl ether. Yield: 7.8 g, melting point: 268°-70° C.

1. filtrationfiltered while hot
2. additionIce-water is then added to the filtrate
3. customthe precipitated solid is isolated
4. customAfter drying at 110° C.
5. customthe product is recrystallized from glycol monomethyl ether