摘要
应用硝基乙烷与丙烯酸甲酯的Michael加成反应,合成了两种含硝基的酯类化合物4-硝基戊酸甲酯(Ⅰ)和4-甲基-4-硝基庚二酸二甲酯(Ⅱ)。考察了不同碱性催化剂及反应条件对两种产物收率的影响。结果表明,KOH固体对两种产物的形成都有很好的催化作用,当硝基乙烷、丙烯酸甲酯、KOH固体的摩尔比为1∶2.2∶0.05,50℃反应3.5h时,产物Ⅱ的收率可达92.4%;而当硝基乙烷、丙烯酸甲酯、KOH固体的摩尔比为1.5∶1∶0.05,30℃反应2h时,产物Ⅰ的收率可达66.9%。用元素分析及红外光谱分析确认了所合成产物的组成和结构。
Two kinds of nitro-containing carboxylic esters such as methyl 4 -nitrovalerate(Ⅰ) and dimethyl 4-methyl-4- nitropimelate(Ⅱ) were prepared by Michael addition of nitroethane to methyl acrylate with four kinds of base as catalysts. The effects of different kinds of basic catalysts and reaction conditions on the yield of the two products were examined. The result showed that solid KOH as the catalyst had best catalyzation for producing the two products. The yield of product (Ⅱ) could reach 92.4 % when the raw materials reacted at 50℃ for 3.5 hours with the molar ratio of nitroethane, methyl acrylate to solid KOH 1 : 2.2:0.05.The yield of product (Ⅰ) could reach 66. 9 % when the raw materials reacted for 2 hours at 30℃ with the molar ratio of nitroethane, methyl acrylate to solid KOH 1.5:1:0.05.The products were characterized by IR and elemental analysis.
出处
《精细石油化工进展》
CAS
2006年第9期51-54,共4页
Advances in Fine Petrochemicals
关键词
氢氧化钾
MICHAEL加成
硝基酯
合成
十六烷值改进剂
potassium hydrate,Michael addition,nitro-containing carboxylic ester, synthesis, cetane number improver