Thiazole derivative preparation method
A technology of derivatives and thiazoles, applied in the field of preparation of thiazole derivatives, can solve the problems of high cost, unsuitable for industrial scale production and the like, and achieve the effects of simple operation, large implementation value and economic benefits, and mild reaction conditions
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Embodiment 1
[0024] Add 500ml of 2-methyl-tetrahydrofuran, water (KF) ≤ 0.05% to a dry and clean 1L four-necked bottle, start stirring, then add 50.0g (0.21mol) of the bromide compound of formula 2, stir for 10min and then cool down to -15 ~-5°C, temperature control -15~-5°C Add 137.9g (0.27mol) of isopropylmagnesium chloride Grignard reagent (Formula 3) to the system dropwise, keep warm for 0.5h, take samples and TLC to track the raw materials without remaining, and then cool down the reaction system To -20~-10℃, gas CO is introduced under the temperature control liquid surface 2 Insulate and react for 3 to 6 hours, take samples to track until the intermediate is no longer converted, add 200ml of tap water dropwise to the system, stir for 0.5h, filter and separate the liquids, extract the water phase twice with 250ml of dichloromethane, keep the water phase, and dilute the water Cool down to 10-15°C, add 27.7g (0.27mol) concentrated hydrochloric acid dropwise, adjust pH=1-2 by adding co...
Embodiment 2
[0027] Add 500ml of toluene and water (KF)≤0.05% to a dry and clean 1L four-necked bottle, start stirring, then add 50.0g (0.21mol) of the bromide compound of formula 2, stir for 10min and then cool down to -15~-5℃, Control the temperature at -15~-5℃, add 124.2g (0.24mol) of isopropylmagnesium chloride Grignard reagent (Formula 3) to the system dropwise, keep it warm for 0.5h, take a sample and TLC to track the raw materials, and then cool down the reaction system to -20~- 10°C, gas CO is introduced under the temperature-controlled liquid surface 2 Insulate and react for 3 to 6 hours, take samples to track until the intermediate is no longer converted, add 200ml of tap water dropwise to the system, stir for 0.5h, filter and separate the liquids, extract the water phase twice with 250ml of dichloromethane, keep the water phase, and dilute the water Cool down to 10-15°C, add 27.7g (0.27mol) concentrated hydrochloric acid dropwise, adjust pH=1-2 by adding concentrated hydrochlori...
Embodiment 3
[0030] Add 500ml of tetrahydrofuran and water (KF)≤0.05% to a dry and clean 1L four-necked bottle, start stirring, then add 50.0g (0.21mol) of the bromide compound of formula 2, stir for 10min and then cool down to -15~-5℃, Control the temperature at -15~-5℃, add 162.0g (0.32mol) of isopropylmagnesium chloride Grignard reagent (Formula 3) to the system dropwise, keep it warm for 0.5h, take a sample and TLC to track the raw materials, and then cool the reaction system to -20~- 10°C, gas CO is introduced under the temperature-controlled liquid surface 2 Insulate and react for 3-6 hours, take samples to track until the intermediate is no longer converted, raise the temperature to 35-45°C, concentrate to remove tetrahydrofuran, add 200ml of tap water dropwise to the system, stir 200ml of ethyl acetate for 0.5h, filter and desalt, then separate the liquid, water Then use 250ml dichloromethane to extract twice, keep the water phase, cool the water phase to 10-15°C, add 27.7g (0.27mo...
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