1-（3，5-二甲基苯基）-1-［（1S，4S）-1，7，7-三甲基双环［2．2．1］庚烷-2-基］肼的合成工艺改进

摘要

3,5-Dimethyl-N-[(1S,4S)-1,7,7-trimethylbicyclo[2.2.1] heptan-2-ylidene] aniline(1) was prepared by microwave-assisted condensation of 3,5-dimethylaniline with 2-camphonone.1-(3,5-Dimethylphenyl)-1-[(1S,4S)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-yl]hydrazine in total yield of 70.4%was synthesized by reduction of 1 by NaBH4 followed by amination with hydroxylamine-O-sulfo-nic acid.The structure was confirmed by 1 H NMR and ESI-MS.%以3，5-二甲基苯胺和2-莰酮为起始原料，在微波促进下，经缩合反应制得N-（3，5-二甲基苯基）-1-（1S，4S）-1，7，7-三甲基二环[2．2．1]庚烷-2-亚胺（1）；1经硼氢化钠还原后再与羟胺-O-磺酸经胺化反应合成了1-（3，5-二甲基苯基）-1-[（1S，4S）-1，7，7-三甲基双环[2．2．1]庚烷-2-基]肼，总收率70．4％，其结构经1H NMR和ESI-MS确证。