Preparation method of medetomidine
A technology of medetomidine and trimethylsilimidazole, which is applied in the field of drug synthesis, can solve the problems of difficult recycling, large amount of catalyst, and difficult recovery of solvents, and achieve the effect of reducing solvent loss and emission
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[0021] Example 1
[0022]
[0023] The installation of a mechanical stirrer, internal thermometer, dropping funnel, the reaction flask has invested trifluoromethylphenyl 100g, sulfate - 1.68 g of silica gel (Ref. Tetrahedron Letters, 2007,48,3783-3787 Preparation method), the internal temperature drop to -10 deg.] C, and then added dropwise a solution of trimethylsilyl imidazole 16.83gN- trifluoromethyl and 100g of toluene at this temperature, stirred for 30 min after addition; was slowly added dropwise a 16.87g1- (1- chloroethyl) trifluoromethyl-2,3-xylene and 136g of toluene solution, in this case within the control temperature -10 ~ -5 ℃, after completion of the dropwise addition, stirring was continued for 4 hours at this temperature, and thin layer chromatography (TLC ) monitoring the reaction progress; after the completion of the reaction, vacuum filtration, and the filter cake was rinsed to 10g trifluoromethylphenyl. The filter cake (catalyst) was dried in vacuo and then ...
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[0026] Example 2
[0027]
[0028] The installation of a mechanical stirrer, internal thermometer, dropping funnel, the reaction flask has invested trifluoromethylphenyl 100g, Amberlyst 15 cation exchange resin 2.81 g, the inner temperature was lowered to -5 deg.] C, and then added dropwise at this temperature by a 16.83 gN- trimethylsilyl imidazole and trifluoroacetic 100g of toluene solution after complete addition stirring 30min. Was slowly dropwise added 16.87g 1- (1- chloroethyl) -2,3-xylene and 136g of toluene solution of trifluoromethyl, in this case within the control temperature -5 ~ 0 ℃, after completion of the dropwise addition, this stirring was continued at temperature for 7 hours, and thin layer chromatography (TLC) monitoring the reaction progress; after the reaction is completed, vacuum filtration, and rinsed in a 10g trifluoromethylphenyl filter cake (catalyst) Natural dry spare ; the filtrate was heated to 50 deg.] C and incubated for 1 hour, allowed to cool wa...
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[0030] Example 3
[0031]
[0032] To the reaction bottle mounted, the built-in temperature meter, the drip funnel, the HZSM-5 molecular sieve 3G, the temperature dropped to 0 ° C, then at this temperature, 15.83 GN-Trimethium The solution of the base silicon imidazole and 100 g chlorobenzene is added after the addition is 30 min; slowly added a solution of 16.87 g 1- (1-chlorthyl) -2,3-xylene and 136 g of chlorobenzene, at this time When the temperature did not exceed 5 ° C, stirring was continued for 8 hours at this temperature, and the reaction process was monitored by a thin layer chromatography (TLC); after the reaction was completed, the filtration was filtered under reduced pressure, and filtered with 10 g of chlorobenzene Pie, filter cake (catalyst) naturally drying back with a small amount of diethyl ether; heating the filtrate to 50 ° C and holding for 1 hour, naturally cooled, 30 ml × 3, saturated saline 30 ml of water, anhydrous sodium sulfate Dry reduced pressure dist...
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