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作 者:姚立红[1] 齐立权[1] 陈新[1] 苏长安[2] 景逵[2]
机构地区:[1]辽宁大学化学系 [2]辽宁大学分析测试中心
出 处:《化学试剂》1997年第4期206-209,217,共5页Chemical Reagents
摘 要:报道了新型手性衍生化试剂2-甲氧基-2-三氟甲基-2-苯基乙胺(MTPEA)的合成及拆分方法。以溴苯和三氟乙酸为主要原料通过3步反应合成了外消旋的MTPEA,合成总收率为53.3%。以光学活性酒石酸为拆分剂在甲醇中通过化学拆分得到光学纯度分别为95.1%和95.8%的S-(+)-MTPEA和R-(-)-MTPEA,拆分总收率为24.4%。并进一步研究了MTPEA分子中碳和氟原子间的偶合作用,归属了分子中各碳原子的化学位移信号。he methods of synthesis and resolution of 2 methoxy 2 trifluoromethyl 2 phenylethylamine(MTPEA) as a novel chiral derivatizing agent were studied D,L MTPEA was prepared with a total yield of 53 3% from bromobenzene and trifluoroacetic acid via three steps The R (-) MTPEA and S (+) MTPEA were obtained with 95 8% O P and 95 1% O P by the resolution of D,L MTPEA using optically active tartaric acid as the resolution agent in methanol(total resolution yield 24 4%) The coupling action between carbon and fluorine atoms was discussed, 13 CNMR chemical shifts were assigned
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