Zhou Yu-han
2004
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Journal
Fine chemicals
Abstract
2,6-Diethylphenylazomethin(Ⅰ) is the important intermediate of N-alphahaloalkylanilide herbicide.Its quality is key to the purity and yield of the end-product.High-grade Ⅰ can be made by reaction of 2,6-diethylaniline in a tubular reactor with a formaldehyde alcohol complex,gotten by contacting parafomaldehyde with alcohol in the presence of catalytic amount of a base.The reaction is carried out in xylene solvent,which forms an azeotrope with alcohol and the water of reaction during vacuum distillation.The reaction is completed when the moisture content of the distillate is less than 0.005 mol/L.Ⅰ was collected under a pressure of 7277 Pa at 104~105 ℃.The purity can reach 98% by gas-chromatographic analysis.