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描述了一种有效的环境友好的“一锅煮”法合成13-乙酰基-9-甲基-11-羰基-8-氧代-10,12-二氮杂三环[7．3．1．0~(2,7)]十三碳-2,4,6-三烯。该法用廉价易得的溴化镁作催化剂,在无溶剂存在下,由起始原料水杨酸,乙酰丙酮和脲通过Biginelli缩合反应伴随着分子内的Michael加成反应一步完成。用核磁共振氢谱、碳谱、飞行时间质谱以及红外光谱数据表征了产物的结构为一氧桥多环化合物,而不是带有自由羟基的二氢嘧啶酮。最后由质谱给出的精确质量及其所代表的元素组成推出了该化合物的质谱裂解途径。
Describes an efficient, environmentally friendly “one-pot” synthesis of 13-acetyl-9-methyl-11-carbonyl-8-oxo-10,12-diazatricyclo [7.3.1.0 ~ (2,7)] trideca-2,4,6-triene. The method uses inexpensive and readily available magnesium bromide as a catalyst in the presence of a solvent, and the starting materials salicylic acid, acetylacetone and urea by Biginelli condensation reaction accompanied by an intramolecular Michael addition reaction is completed in one step. The structure of the product was characterized by 1H NMR, GC, FT-IR and FT-IR. The structure of the product was the mono-bridged polycyclic compound rather than the dihydropyrimidone with free hydroxyl. Finally, the exact mass given by mass spectrometry and the elemental composition it represents have led to the mass spectrometric cleavage pathway of this compound.