Preparation of cis-2-(2,4- dichlorophenyl)-2-([1,2,4]- triazole-1-methyl )-[1,3] dioxolane -4-Methyl methanesulfonate
A technology of methyl methanesulfonate and dichlorophenyl, applied in the field of pharmaceutical synthesis, can solve problems such as easy to cause combustion or explosion, unavoidable deep bromination, complicated post-processing, etc., and achieve the effect of avoiding column chromatography
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[0019] The following examples describe the invention in detail. However, these examples are by no means limiting the protection scope of the present invention.
[0020] (1) Synthesis of 2-bromo-1-(2,4-dichlorophenyl)ethanone
[0021] Put 150g (1.12mol) of anhydrous aluminum trichloride into a 500mL three-necked flask, add 147g (1.00mol) of m-dichlorobenzene, stir at room temperature, and slowly add 201g (1.00mol) of bromoacetyl bromide dropwise Continue to stir at room temperature for 30 minutes, slowly raise the temperature to 50-55°C, and stir at this temperature for 5 hours, pour the reaction solution into ice water to freeze, cool to room temperature, and extract twice with 500mL dichloromethane, The dichloromethane extracts were combined, washed with water until neutral, dried over anhydrous sodium sulfate, the solvent was recovered by filtration, and the residue was reconstituted to obtain 240 g of a white irritating solid with a yield of 90.0%.
[0022] (2) Synthesis ...
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