69673-92-3Relevant articles and documents
Access to α,α-dihaloacetophenones through anodic C[dbnd]C bond cleavage in enaminones
Zhang, Zhenlei,Yang, Jiusi,Wu, Kairui,Yu, Renjie,Bu, Jiping,Huang, Zijun,Li, Shaoke,Ma, Xiantao
supporting information, (2021/12/20)
We have developed a method to synthesize α,α-dihaloketones under electrochemical conditions. In this reaction, the Cl- or Br- is oxidized to Cl2 or Br2 at the anode, which undergoes two-step addition reactions with the N,N-dimethyl enaminone, and finally breaks C[dbnd]C of the N,N-dimethyl enaminone to generate α,α-dihaloketones. The electrosynthesis reaction can be conveniently carried out in an undivided electrolytic cell at room temperature. In addition, various functional groups are compatible with this green protocol which can be applied simultaneously to the gram scale without significantly lower yield.
Production method of 2-(4-bromomethyl phenyl)propionic acid
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Paragraph 0016; 0022; 0025, (2020/03/06)
The invention discloses a production method of 2-(4-bromomethyl phenyl)propionic acid. An adopted ionic liquid catalyst can be recycled and used, no molten aluminum trichloride is generated, a material does not need to be washed for multiple times, only layered extraction needs to be conducted, then a required product can be obtained, aluminum trichloride and triethanolamine salt ionic liquid is used, thus environmentally friendliness is achieved, the cost is also saved, and that is, an original cumbersome process is simplified. An original bromination reaction in a glass kettle is changed toa cooling glass pipeline circulation-type bromination reaction in the kettle, through the glass pipeline type reaction, the contact area of the material and light is increased, through circulation, the situation that the material is gathered on the illumination surface, and consequently light illumination is affected is avoided, thus the reaction efficiency is higher, the reaction time is shortened, the occurrence of a side reaction is controlled, and the product purity is higher.
Method for synthesizing loxoprofen sodium medicine intermediate 1-p-methylphenyl-2-chloro-acetone
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Paragraph 0015; 0016, (2016/11/14)
The invention relates to a method for synthesizing a Loxoprofen sodium medicine intermediate 1-p-methylphenyl-2-chloro-acetone. The method comprises the following steps: (i) adding 2.4 to 2.43 mol of stannous chloride and 1.2L of methylbenzene to a reaction vessel provided with a stirrer, a thermometer, a reflux condenser and a dropping funnel, reducing the temperature of the solution to 2 to 5 DEG C, and dropwise adding 2.1 mol of 2-chloride propionamide, wherein the dropwise adding time is controlled within 3h to 4h; maintaining the stirring speed to be 180rpm to 210 rpm for 9h to 10h, pouring the reactant to 2L of sodium chloride solution, reducing the temperature of the solution to 2 to 4 DEG C, separating an organic layer out, extracting a water layer with methylbenzene for 3 to 6 times, merging the organic layers, washing with a sodium carbonate solution and a salt solution in sequence, carrying out reduced-pressure distillation, recovering a solvent to obtain an oily matter, reducing the temperature of the solution to 12 to 15 DEG C and separating solid out, adding a cyclohexane solution, maintaining the stirring speed to be 200rpm to 230rpm, carrying out suction filtering, and dehydrating with a dehydrating agent to obtain white solid 1-p-methylphenyl-2-chloro-acetone.