摘要
联合运用“相转移催化技术”和“连续反应”法 ,以 60 %~ 97%的收率合成了 1 6个未见文献报道的硫代磷酸酯 ,通式为 CH3O(Xn-C6 H5- n O) P(S) OCH2 C CH。用元素分析、IR和 1 H NMR进行了结构表征 ,并对相转移催化剂 TEBAC和 TBAB的效用做了优化研究。生物活性实验结果表明 ,施药浓度为 0 .0 2 5 %时 ,部分目标化合物 5、 4 和 7对蚜虫的致死率分别为 1 0 0 %、70 %和 66.5 %。
Sixteen O substituted aryl O methyl O propargyl thiophosphates were synthesized via tandem reaction in dichloromethane by PTC in the presence of triethyl ammonium chloride (TEBAC) and/or tetrabutyl ammonium bromide(TBAB) and triethylene diamine. At condition of m (TEBAC)∶ m (TBAB)=1:1, pH=9~10, 25~35 ℃, 2 5~3 h thiophosphates were obtained in yields of 60%~97%. The structures of the compounds were characterized by elemental analysis, IR and 1H NMR spectroscopy. The compound Ⅲ 5 ( O 4 nitrophenyl O methyl O propargyl thiophosphate) showed an excellent insecticidal activity against aphid nearly 100% in dosage of 0 025%.
出处
《应用化学》
CAS
CSCD
北大核心
2002年第9期870-873,共4页
Chinese Journal of Applied Chemistry
基金
国家计划委员会攻关项目 (97-5 63 -0 2 -0 5 )资助课题