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2,2-二甲基-1,3-丙二胺(1)是有机中间体,国内市场尚无供应,文献报道可由2,2-二甲基-1,3-二硝基丙烷(2)加压催化还原合成。我们采用铁屑和盐酸进行还原,方法简便,易于推广。合成2所用催化剂以吡啶收率最低,哌啶和二乙胺相仿,但二乙胺用量较大。 .实验部分一、2,2-二甲基-1,3-二硝基丙烷(2) 将丙酮11 ml(0.15 mol)、硝基甲烷24 ml(0.45mol),哌啶3 ml(0.O3mol)加入烧瓶中,搅拌,加热回流反应16 h,用2 mol/L盐酸调至pH 2,分出油层,水层用氯仿提取,合并油层及提取液,用无水硫酸钠干燥,回收氯仿后减压蒸馏,收集124～128℃/2.1 kPa(16 mmHg)的馏份15 g,产率61.7％,mp 89～90℃(文献mp 89～90℃)。
2,2-dimethyl-1,3-propanediamine (1) is an organic intermediate, there is no domestic market supply, reported in the literature from 2,2-dimethyl-1,3-dinitropropane ) Pressurized catalytic reduction synthesis. We use iron scrap and hydrochloric acid for reduction, the method is simple and easy to popularize. The catalyst used in the synthesis of 2 had the lowest yield of pyridine, while the piperidine and diethylamine were similar, but the amount of diethylamine was relatively large. Experimental Part One 2,2-Dimethyl-1,3-dinitropropane (2) Acetone 11 ml (0.15 mol), nitromethane 24 ml (0.45 mol), piperidine 3 ml (0. O3mol) was added to the flask, stirred and heated to reflux for 16 h, with 2 mol / L hydrochloric acid adjusted to pH 2, the separation of the oil layer, the aqueous layer was extracted with chloroform, the combined oil layer and the extract, dried over anhydrous sodium sulfate, chloroform After the distillation under reduced pressure, 15 g of a fraction of 124 to 128 ° C / 2.1 kPa (16 mmHg) was collected in a yield of 61.7%. Mp 89-90 ° C (mp 89-90 ° C).