丙酮肟氧化偶联合成2,3-二甲基-2,3-二硝基丁烷反应的研究

Synthesis of 2,3-Dimethyl-2,3-dinitrobutane by Oxidative Coupling of Acetone Oxime

以丙酮肟为原料,在改性TS-1(钛硅分子筛)催化剂催化下,可用H2O2氧化偶联合成2,3-二甲基-2,3-二硝基丁烷(DMNB).在此基础上以丙酮为原料,在改性TS-1催化剂催化下,一锅法进行丙酮氨肟化和氧化偶联反应可制备收率43.2%的DMNB.该方法简便易操作,操作安全.产物结构经1H NMR,13C NMR表征.

2,3-Dimethyl-2,3-dinitrobutane（DMNB） was prepared by oxidative coupling of acetone oxime with H2O2over the modified TS-1 catalyst.In one-pot operation,the ammoximation of acetone followed by catalytic oxidative coupling over TS-1 produced the DMNB with yield of 43.2%.The operation is simple and safe.The structures of products were identified by 1H NMR and13C NMR spectra.