摘要
以邻氰基氯苄与亚磷酸三乙酯反应得到邻氰基苄基膦酸二乙酯,再与芳醛(苯甲醛、邻氯苯甲醛、间氯苯甲醛、对甲砜基苯甲醛和2-噻吩甲醛)在甲醇钠和N,N-二甲基甲酰胺中经Wittig-Horner反应合成了5个邻氰基二苯乙烯类化合物,收率83.8%～93.1%,其中4个为未见报道的新化合物。所有产品均经熔点、高效液相色谱和核磁共振氢谱等表征。反应的优化条件为邻氰基苄基膦酸二乙酯、芳醛、甲醇钠的摩尔比为1.02:1.00:1.08,N,N-二甲基甲酰胺80 mL,反应温度30℃、时间5～6 h(醛投料0.24 mol)。所用方法具有收率稳定、操作简便、原料成本低廉等优点。
The preparation and characterization of 5 o-cyanostilbenes from o-cyanobenzyl chloride、triethyl phosphite、aromatic aldehydes in N,N-dimethyl formamide via Wittig-Horner reaction are reported.The yields range from 83.8% to 93.1%,among them four compounds has not been previously reported.The products were characterized by melting points,TLC,HPLC and 1H-NMR spectroscopy.Optimal reaction conditions are: o-cyanobenzyl diethylphosphite:aldehyde:sodium methoxide(molar ratio) 1.02:1.00:1.08,DMF 80 mL,temperature 30 ℃,time 5~6 h(with 0.24 mol aldehyde).The reported method has the advantages of reliable and high yields,simple operations,cheap and readily available raw materials.
出处
《化工生产与技术》
CAS
2011年第3期28-31,70,共4页
Chemical Production and Technology
