1–(3–硝基–2–吡啶)–1H–苯并三唑的合成与表征

Synthesis and Characterization of 1-(3-Nitro-2-Pyridyl)-1H-Benzotriazole

以苯并三氮唑和2–氯–3–硝基–吡啶为原料,合成出1–(3–硝基–2–吡啶)–1H–苯并三唑。采用元素分析、核磁共振光谱等手段鉴定了目标产物结构,并用DSC测定了产物的熔点。考察了反应溶剂、溶剂用量、缚酸剂种类、缚酸剂用量对该反应收率和产品纯度的影响。确定的最佳工艺条件为:以工业乙醇为反应溶剂,溶剂与反应物的原料比为200 mL∶0.1 mol,Na2CO3为反应缚酸剂,缚酸剂与苯并三氮唑的摩尔比为1∶1,反应时间为12 h。

The 1-（3-nitro-2-pyridy1）-lH-benzotriazole was synthesized by using benzotriazole and 2-chloro-3- nitropyridine as raw materials. The structure of the target product was characterized by using element analysis, nuclear magnetic resonance spectrum and so on, and the melting point of the product was determined by using DSC. The influence of reaction solvent, solvent amount, type and amount of deacidification agent on reaction yield and product purity was investigated. The defined optimal process conditions are as follows： using industrial ethanol as reaction solvent, the ratio of solvent to reactants is 200 mL ： 0.1 tool, using Na2CO3 as reaction deacidification agent, the molar ratio of deacidification agent to benzotriazole is 1 ： 1, the reaction time is 12 h.