21327-86-6Relevant articles and documents
Method for preparing polysoproxil intermediate
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Paragraph 0034; 0088-0093, (2021/11/26)
The method comprises the following steps: (1). A hydrogen chloride salt of 2 - chlorine -6 - methylaniline compound 1 is prepared by taking 2 - chlorine -6 - methylaniline compound 1 as a raw material in a suitable solvent, and then subjected to diazotization reaction with a nitration reagent aqueous solution to obtain the diazonium salt 2 - chloro -6 - methylaniline. The iodine-containing reagent is reacted with an iodo reagent to obtain 3 -chloro -2 -iodotoluene compound 2. (2), the compound 2 is reacted with the reactant cyanide to give 2 -chloro -6 -iodo-benzonitrile compound 3. (3), the compound 3 undergoes a hydrolysis reaction to obtain 2 - chloro -6 - methyl benzoic acid compound 4, and the reaction equation is as follows. The method has the advantages of cheap and easily available raw materials, high reaction conversion rate, simplicity and rapidness, mild and controllable reaction conditions, mild reaction conditions, high yield of the obtained product, easy separation and purification, high purity and easy industrial mass production.
Flow carbonylation of sterically hindered ortho-substituted iodoarenes
Mallia, Carl J.,Walter, Gary C.,Baxendale, Ian R.
supporting information, p. 1503 - 1511 (2016/08/02)
The flow synthesis of ortho-substituted carboxylic acids, using carbon monoxide gas, has been studied for a number of substrates. The optimised conditions make use of a simple catalyst system compromising of triphenylphosphine as the ligand and palladium acetate as the pre-catalyst. Carbon monoxide was introduced via a reverse "tube-in-tube" flow reactor at elevated pressures to give yields of carboxylated products that are much higher than those obtained under normal batch conditions.
Process development of an inherently safer oxidation: Synthesis of 2-chloro-6-methylbenzoic acid in the R411 manufacturing process
Lopez, Flavio Chavez,Shankar, Ashish,Thompson, Maethonia,Shealy, Brandon,Locklear, Dobbert,Rawalpally, Thimma,Cleary, Thomas,Gagliardi, Charles
, p. 1003 - 1008 (2012/12/26)
Many oxidation reactions can be hazardous when run on large scale. The manufacturing process for the production of R411, a developmental compound indicated for the treatment of asthma, includes the oxidation of 2-chloro-6-methylbenzaldehyde to the corresponding carboxylic acid. The use of sodium chlorite in this transformation was efficient and economical, but there were safety concerns regarding the use of hydrogen peroxide to scavenge unwanted hypochlorite, which was generated as a byproduct of the reaction. During the development of the R411 manufacturing process, an inherently safer oxidation system was discovered using a stoichiometric quantity of dimethyl sulfoxide (DMSO) as scavenger. The new process provided equivalent yields and purities to the hydrogen peroxide procedure, thus maintaining the economic viability of the process. The developed process was demonstrated in fixed equipment on a 300 gal scale.