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以富马酸为原料制备富马腈的新工艺研究
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作者 林韦康 江晓明 +1 位作者 武立靖 归晨秋 《浙江化工》 CAS 2020年第1期14-19,共6页
为开发一种工业化可行、操作简便、职业危害性小的富马腈生产工艺,本文独辟蹊径,以富马酸为起始原料,经酰胺化、脱水、蒸馏、打浆工序可稳定制得气相含量高于99.90%的目标产物。当n(20%氨水):n(富马酸)=2.05:1,反应温度为120℃,反应压力... 为开发一种工业化可行、操作简便、职业危害性小的富马腈生产工艺,本文独辟蹊径,以富马酸为起始原料,经酰胺化、脱水、蒸馏、打浆工序可稳定制得气相含量高于99.90%的目标产物。当n(20%氨水):n(富马酸)=2.05:1,反应温度为120℃,反应压力为0.30 MPa时,酰胺化效果最好;用1.09 eq氯化亚砜分两阶段对富马酸酰胺进行脱水时,脱水效率最高;脱水后的料液加入少量对苯二酚作为阻聚剂,先回收溶剂二甲苯,再继续蒸馏获得富马腈粗品;最后富马腈粗品用正庚烷于70℃~80℃打浆2 h,可得到气相含量为99.92%,熔点为95.3℃~95.4℃,核磁氢谱特征峰正确的富马腈成品,总收率为93.2%。 展开更多
关键词 富马腈 反丁烯二腈 酰胺脱水 羧酸酰胺化
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Ru(Ⅱ)-catalyzed ortho-amidation and decarboxylation of aromatic acids: a versatile route to meta-substituted N-aryl benzamides 被引量:1
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作者 Xian-Ying Shi Xue-Fen Dong +3 位作者 Juan Fan Ke-Yan Liu Jun-Fa Wei Chao-Jun Li 《Science China Chemistry》 SCIE EI CAS CSCD 2015年第8期1286-1291,共6页
Carboxylate as a promising and valuable directing group has attracted a great deal of attention.However,employing it as a traceless direction group has rarely been reported.We developed the ruthenium-catalyzed amidati... Carboxylate as a promising and valuable directing group has attracted a great deal of attention.However,employing it as a traceless direction group has rarely been reported.We developed the ruthenium-catalyzed amidation of substituted benzoic acids with isocyanates via directed C–H functionalization followed by decarboxylation to afford the corresponding metasubstituted N-aryl benzamides,in which the carboxylate serves as a unique,removable directing group.Notably,this protocol can provide an efficient alternative to access meta-substituted N-aryl benzamides,which are much more difficult to prepare than ortho-substituted analogues. 展开更多
关键词 AMIDES DECARBOXYLATION AMIDATION C-H functionalization homogeneous catalysis
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Iron-catalyzed aerobic oxidative amidation of tertiary amines with carboxylic acids
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作者 Lina Ma Yuanming Li Zhiping Li 《Science China Chemistry》 SCIE EI CAS CSCD 2015年第8期1310-1315,共6页
An oxidative amidation of tertiary amines with carboxylic acids has been developed in the presence of FeC13- 6H20 as catalyst and oxygen as oxidant. A variety of tertiary amides were obtained in good to excellent yiel... An oxidative amidation of tertiary amines with carboxylic acids has been developed in the presence of FeC13- 6H20 as catalyst and oxygen as oxidant. A variety of tertiary amides were obtained in good to excellent yields from inexpensive and readily available reagents. The possible reaction pathways were investigated. 展开更多
关键词 AMIDATION tertiary amine carboxylic acid iron catalysis OXIDATION
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