Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 107512-34-5, name is 4-Chloro-3-methoxy-2-methylpyridine. A new synthetic method of this compound is introduced below., COA of Formula: C7H8ClNO
Step 1, the 12 parts by weight of the acidic phosphotungstic acid dissolved in water prepared for mass concentration 25% phosphotungstic acid solution;Step 2, weighing 220 parts by weight of 4 – chloro -3 – methoxy -2 – methyl pyridine, slowly added under stirring step 1 bedded phosphotungstic acid solution, stirring to complete mixing, heating in water bath temperature is raised to 87 C, dropwise 350 parts by weight of the mass concentration is 35% hydrogen peroxide, hydrogen peroxide is accelerated-rate drop 60 parts by weight/hours; then in 85 C lower heat insulating 5 hours, to obtain the reaction solution;Step 3, the reaction cooling to 30 C is added after a dilute alkali solution (mass concentration 12% sodium hydroxide aqueous solution) adjusted to pH 7 – 9, then the dichloromethane extraction, water washing extract in neutral, adds anhydrously Na2SO4Drying, at a temperature of 35 – 45 C, pressure 0.06 – 0.08 mpa evaporating the dichloromethane under reduced pressure, to obtain 230.2 parts by weight of the obtained 4 – chloro -3 – methoxy -2 – methyl pyridine – N – oxide; high performance liquid chromatogram of the product, the product appearance time is as shown in Figure 7, 3.740 min, according to the appearance time can be qualitative verification product; product 4 – chloro -3 – methoxy -2 – methyl pyridine – N – oxide of high purity, according to the area of the yield of the product is calculated unitary method 95%.
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Reference:
Patent; Anhui Jin He Industrial Co., Ltd.; Chuzhou College; Xia Jiaxin; Wang Yonggui; Ge Xiutao; Geng Qingbao; Yang Zhijian; (10 pag.)CN107129466; (2017); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem