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Nitration of toluene with 65% nitric acid over MoO3/SiO2 as catalyst
相关领域
化学工程
材料科学
相(物质)
有机化学
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其它 | (NH4)6Mo7O244H2O, 1.83 g, dissolved in 15 mL H2O2, was deposited on 8.5 g of 0.5-1.0-mm SiO2gel, dried 24 h at 110°C, and calcined 18 h at 550°C in air stream to yield 10 g 15% MoO3/SiO2 catalyst. This 10 g catalyzed nitration of 0.37 g C6H5CH3in 22 mL CCl4 with 1.85 g aq. 65% HNO3 for 2.5 h at room temp. The products were filtered, washed (NaHCO3, H2O), dried over MgSO4, and gas chromatographed. The C6H5CH3/HNO3ratios studied were 1:1-1:10; at 1:4, the yield was max. at 52.7% (vs. the 7% with no catalyst used); at 1:10, the yield was 32%, same as with no catalyst. As the MoO3 in the catalyst was increased (to 50 wt.%), the yield fell. The 15% MoO3/SiO2 was best as catalyst. It was regioselective, favorable to the mononitro-derivatives and to the p-nitro product The para-to-ortho ratio was invariably ca. 0.7. |
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