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机构地区:[1]大连理工大学精细化工国家重点实验室,大连116012
出 处:《染料与染色》2004年第5期284-286,共3页Dyestuffs and Coloration
摘 要:以苯酚为原料通过烷基化、醛基化、溴化或硝化等单元反应设计合成了5-叔丁基水杨醛(收率:74.4%、m/z177为M-1峰)、3-溴-5-叔丁基水杨醛(收率:65.7%、m.p.88~89℃、m/z:256 M-1峰)、3-硝基-5-叔丁基水杨醛(收率:59.1%、mp:90℃~91℃、m/z :222M-1峰).在甲氧基镁的作用下采用多聚甲醛进行醛基化的反应收率可达65%以上,产品纯度较高,反应条件对醛基化过程影响较大,在无水条件下进行醛基化反应对提高醛基化收率是有益的.用NMR和MS对化合物进行了表征.5-tert-Butyl-salicyialdehyde (yield: 74.4%), 3-bromo-5-tett-butyl-salicylaldehyde (yield: 91%, b.p. 83℃/132Pa)and 3-nitro-5-tert-butyl-salicylaldehyde (yield: 59%, m.p. 90-91 ℃) were synthesized from phenol via alkylation. hydroformylation, bromination or nitration. Satisfactory yields (>65%) and higher purity by hydroformylation were achieved by using magnesium methoxide and paraformaldehyde. The results of hydroformylation were affected by the reaction conditions appreciably. And the yields were improved when the reactions were carried out under N2. These compounds were characterized by 1H-NMR, 13C-NMR and Mass spectra.
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