Micro-channel reactor and method for preparing dapagliflozin intermediate based on reactor
A technology for microchannel reactors and intermediates, applied in chemical instruments and methods, chemical/physical/physicochemical reactors, preparation of sugar derivatives, etc., can solve the problem of no obvious optimization of reaction steps and low safety of n-butyllithium , Low reactivity of raw materials and other issues, to achieve the effect of safe and environmentally friendly synthesis process, mild reaction conditions, and shortened reaction time
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Embodiment 1
The present invention provides such as Figure 1-Figure 2 The microchannel reactor shown includes
Reaction part A1, which includes reaction chamber A15;
Reaction part B2, which includes reaction chamber B23;
a reaction part C3, which includes a reaction chamber C33;
The reaction chamber A15, the reaction chamber B23 and the reaction chamber C33 are communicated;
Extraction tower 4 is arranged at the outlet of reaction chamber C33;
The jet mill is connected with the reaction part A1, the reaction part B2 and the reaction part C3 through the metering pump 5;
The catalyst packing pipe 6 is arranged in the airflow pulverizer. The catalyst packing pipe 6 includes a sieve hole 61 and an airflow channel 62, and the sieve hole 61 is filled with catalyst.
[0023] Preferably, the reaction part A1 further comprises a cooling tower 11, a metering pump 12, a cooling tower 2 13 and a metering pump 2 14, the cooling tower 11 and the metering pump 1 12 are connected to the reactio...
Embodiment 2
Dissolve 20g (0.05mol) of 1-chloro-2-(4-ethoxybenzyl)-4-iodobenzene in 100 mL of toluene to prepare a 0.5mol / L solution (reaction solution 1), and then transfer it Carry out -10 ℃ pre-cooling in cooling tower one 11, transfer 50 mL of 1 mol / L isopropylmagnesium chloride / lithium chloride complex (reaction solution 2) to another cooling tower two 13 for -10 ℃ pre-cooling. Cold, wherein the molar ratio of isopropylmagnesium chloride to lithium chloride is 1:1, 23.35g (0.05mol) 2,3,4,6-tetra-0-trimethylsilyl-D-gluconolactone Dissolve in 100 mL of toluene to prepare a 0.5 mol / L solution (reaction solution 3), and mix 100 mL of 36% concentrated hydrochloric acid with 300 mL of methanol (reaction solution 4);
Set the temperature of the microchannel reactor to 0 °C, set the flow rate of metering pump one 12 to 10 mL / min, and set the flow rate of metering pump two 14 to 5 mL / min. 2. Pump into the reaction chamber A15 of the microchannel reactor, set the flow rate of the metering pump ...
Embodiment 3
Dissolve 20g (0.05mol) of 1-chloro-2-(4-ethoxybenzyl)-4-iodobenzene in 100 mL of toluene to prepare a 0.5mol / L solution (reaction solution 1), and then transfer it Pre-cooling at -10°C in cooling tower one 11, transfer 55 mL of 1 mol / L isopropylmagnesium chloride / lithium chloride solution in tetrahydrofuran (reaction solution 2) to another cooling tower two 13 for -10°C pre-cooling. Cold, wherein the molar ratio of isopropylmagnesium chloride to lithium chloride is 1:1, 23.35g (0.05mol) 2,3,4,6-tetra-0-trimethylsilyl-D-gluconolactone Dissolve in 100 mL of toluene to prepare a 0.5 mol / L solution (reaction solution 3), and mix 80 mL of 36% concentrated hydrochloric acid with 320 mL of methanol (reaction solution 4);
Set the temperature of the microchannel reactor to 0°C, set the flow rate of metering pump one 12 to 10 mL / min, and the flow rate of metering pump two 14 to be 5.5 mL / min. 2. Pump into the reaction chamber A15 of the microchannel reactor, set the flow rate of the me...
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