54519-62-9Relevant articles and documents
Method for preparing alpha-nitro ketonic acid from annular anhydride
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Paragraph 0011-0015, (2017/08/30)
The invention discloses a method for preparing alpha-nitro ketonic acid from annular anhydride. The method comprises the steps of sequentially adding 14.8g of phthalic anhydride, 200ml of anhydrous DMSO, 6.1g of nitromethane, 10.1g of triethylamine and 0.1mol of inorganic salt into a 500ml three-neck flask provided with a drying tube, stirring to react at 25 DEG C for 6 hours, carrying out TLC detection in the reaction process, after the raw materials are disappeared, adding 200ml of water, stirring for 10 minutes, acidizing by virtue of 6N hydrochloric acid until the pH is 6.5, extracting by virtue of 500ml of ethyl acetate for three times, combining organic layers, respectively washing by virtue of acetic acid with the pH of 6.5, a sodium acetate buffer solution, water, a saturated saline solution, drying by virtue of anhydrous sodium sulfate, reducing the pressure to recycle ethyl acetate, standing for cooling residual solvents to separate out solids, and filtering, so as to obtain 12.6g of the solids. The method has the characteristics of simplicity, cheap raw materials, low environmental pollution, relatively high yield, easiness in purification and the like.
