丁草胺合成的新工艺

以2,6-二乙基苯胺、甲醛、氯乙酰氯和正丁醇为主要原料,采用一种经济环保的工艺路线,对除草剂丁草胺的合成进行了研究。考察了反应条件对反应结果的影响,获得了较佳的反应条件:烯胺化反应中n(2,6-二乙基苯胺)∶n(甲醛)=1∶1.5,反应温度75~80℃,反应时间2 h;酰化反应中n(2,6-二乙基苯胺)∶n(氯乙酰氯)=1∶1.1,反应温度30~35℃,反应时间1 h;醚化反应中n(2,6-二乙基苯胺)∶n(丁醇)=1∶5.5,反应温度50℃,反应时间5 h。在较佳反应条件下,产品纯度为93%左右,产品收率达87%以上。研究结果表明,该工艺路线是合成除草剂丁草胺的适宜路线,该合成路线反应条件温和、三废少、无设备腐蚀、产品质量分数与收率高。

Study on a New Process for Synthesis of Butachlor

A new process for the synthesis of butachlor was studied by using formaldehyde,2,6-diethylaniline,chloroacetyl chloride and butanol as starting materials.The effects of reaction conditions on results were examined,and the optimum conditions were obtained.In the first step,n(2,6-diethylaniline)∶n(formaldehyde) =1∶1.5,reaction temperature 75~80 ℃,reaction time 2 h.In the second step,n(2,6-diethylaniline)∶n(chloroacetyl chloride)=1∶1.1,reaction temperature 30~35 ℃,reaction time 1 h.In the third step, n(2,6-diethylaniline)∶n(butanol)=1∶5.5,reaction temperature 50 ℃, reaction time 5 h.Under the optimum conditions,the purity and yield of the product were about 93% and 87% respectively.