摘要
二苯胺与三氯化磷在加热条件下相互作用并用水处理后 ,不经乙醇溶出 (分离 ) ,直接用过氧乙酸在含水冰醋酸介质中氧化 ,以 42 %～ 5 0 %的产率合成 10 羟基 5 ,10 二氢苯并磷杂吖嗪 10 氧化物。该方法工艺稳定 ,省去溶剂乙醇 ,减少了反应物用量以及相应的酸碱消耗 ,使目标分子的产率由文献的 37%提高到 40 %以上 ,合成周期由文献的至少 3d缩短到 1～ 2d。对合成的目标分子进行了结构表征 ,结果正确。分析核磁共振结果 。
10-Hydroxy-5, 10-dihydrophenophosphazine-10-oxide was prepared in 42% [similar to] 50% yield by interaction of diphenylamine and phosphorus trichloride at slowly-elevated temperature followed by hydrolysis of the reaction mixture with water, which was then oxidized directly with peroxy acetic acid in glacial acetic acid without separating the reaction mixture by extracting with ethanol. By this new technique, whole process could be easily done within one or two days rather than over three days in literature, the solvent ethanol was deleted, the consume of raw and processing materials used during the synthesis was decreased, and the yield of title compound was raised from 37% in literature to over 40%. Meanwhile, structure of the compound obtained was also identified by surveying its melting point, IR, NMR and mass spectrum, and its more presumable conformation was also advanced by analyzing its 1HNMR.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2001年第8期482-484,492,共4页
Fine Chemicals
