农药科学与管理2024,Vol.45Issue(12) :27-31,40.

O-乙基-S-乙基-O-(3,5,6-三氯-2-吡啶基)磷酸酯的合成

Synthesis of O-Ethyl-S-Ethyl-O-(3,5,6-Trichloro-2-Pyridyl)Phosphates

田俊杰 孙在臣 张斌铨 姚广禹 陈涛 朱恒营
农药科学与管理2024,Vol.45Issue(12) :27-31,40.

O-乙基-S-乙基-O-(3,5,6-三氯-2-吡啶基)磷酸酯的合成

Synthesis of O-Ethyl-S-Ethyl-O-(3,5,6-Trichloro-2-Pyridyl)Phosphates

田俊杰 1孙在臣 2张斌铨 1姚广禹 2陈涛 3朱恒营1
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作者信息

  • 1. 德州绿霸精细化工有限公司,山东 德州 253000;山东恒东生物科技有限公司,山东 平原 253100
  • 2. 山东恒东生物科技有限公司,山东 平原 253100
  • 3. 德州绿霸精细化工有限公司,山东 德州 253000
  • 折叠

摘要

为了研究毒死蜱中转位杂质的含量,及减少毒死蜱合成中该杂质的形成,探究合成O-乙基-S-乙基-O-(3,5,6-三氯-2-吡啶基)磷酸酯的最优工艺参数.以三氯化磷和乙醇为原料,经取代、氨化、缩合、酰化和缩合五步反应合成目标产物.取代、氨化、缩合、酰化和缩合的收率分别为82.3%、90.3%、96.0%、97.1%和96.7%,总收率达到67.0%.实验结果经色谱分析表明:合成的产物气液相面积归一化均可达到98%.

Abstract

The study investigates the content of transposition impurities in chlorpyrifos and explores ways to reduce the formation of the impurity in chlorpyrifos synthesis,the optimal process parameters of synthesizing O-ethyl-S-ethyl-O-(3,5,6-trichloro-2-pyridinyl)phosphate ester were identified.The target product was synthesized in a five-step process,including substitution,ammonification,condensation,acylation and a final condensation,starting from phosphorus trichloride and ethanol.The yields for each step were as follows:substitution 82.3%,ammonification 90.3%,condensation 96.0%,acylation 97.1%,and final condensation 96.7%,leading to an overall yield of 67.0%.Chromatographic analysis showed that the normalized area of the synthesized product reached 98%.

关键词

毒死蜱/乙基氯化物/O-乙基-S-乙基-O-(3,5,6-三氯-2-吡啶基)磷酸酯

Key words

chlorpyrifos/diethyl chlorothiophosphate/O-ethyl-S-ethyl-O-(3,5,6-trichloro-2-pyridyl)phosphates

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出版年

2024
农药科学与管理
农业部农药检定所

农药科学与管理

CSTPCD
影响因子:0.511
ISSN:1002-5480
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