50978-40-0Relevant articles and documents
Preparation and purification method of toxic impurity DCAL of clopidol
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, (2018/04/03)
The invention relates to a preparation and purification method of toxic impurity DCAL of clopidol and belongs to the technical field of preparation of standard medicine products. The preparation and purification method comprises the following steps: firstly carrying out chlorination reaction, i.e., dissolving a solvent and 2,6-dimethyl-4-aminopyridine; then slowly adding a chlorinating agent to carry out chlorination; after reaction is finished, carrying out neutralization and water washing, concentration and crystallization, filtering or direct neutralization and filtering on reaction liquidto obtain a crude DCAL product; purifying the crude DCAL product, adding a mixed solvent of ethanol and ethyl acetate into the crude DCAL product, stirring for dissolving, dripping petroleum ether toprecipitate solids, filtering, carrying out concentration, cooling and precipitation on filtrate, then filtering, and drying solids to obtain a pure DCAL product. The preparation and purification method has the beneficial effects that the reaction temperature is low, the reaction time is short, the side products in reaction are fewer, and the product is easily purified, so that convenience is brought for preparing impurity reference products of the veterinary-drug clopidol.