Stationary bed continuous production method of ezetimibe intermediate
A technology of ezetimibe and its production method, which is applied in the field of pharmaceutical synthesis, can solve the problems of high water content requirements for production equipment and raw materials, difficult recovery of catalysts, difficulty in continuous reaction, etc., and achieve the reduction of environmental pollution and the requirements for production equipment , easy to separate, the effect of continuous large-scale production
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Embodiment 1
[0056] The preparation of embodiment 1 catalyst
[0057] Preparation of CAT-1:
[0058] Weigh 10 g of ZSM-5 molecular sieve (silicon-aluminum ratio Si / Al=25) and add it into 500 mL ammonium nitrate solution with a concentration of 2 mol / L, and stir in a water bath at 80° C. for 2 hours to carry out ion exchange. After repeated exchanges three times, the obtained solid sample was centrifuged, washed three times with deionized water, dried at 100°C, and calcined at 550°C for 4 hours. The obtained H-ZSM-5 molecular sieve sample was designated as CAT-1.
[0059] Preparation of CAT-2:
[0060] Weigh 10 g of ZSM-5 molecular sieve (silicon-aluminum ratio Si / Al=30) and add it into 500 mL ammonium nitrate solution with a concentration of 2 mol / L, and stir in a water bath at 80° C. for 2 hours to carry out ion exchange. After repeated exchanges three times, washed with deionized water three times, dried at 100°C, and calcined at 550°C for 4 hours, the obtained H-ZSM-5 molecular sie...
Embodiment 2
[0067] Embodiment 2 fixed-bed reactor reacts
[0068] Reaction material
[0069] According to the ratio in Table 1, compound A and compound B were respectively dissolved in an organic solvent, the temperature of the system was lowered to below -20°C, and an organic amine and a hydroxyl protecting agent were added to obtain the reaction materials as shown in Table 1.
[0070] Table 1 Reaction raw materials
[0071]
[0072] Note * : A is compound A; B is compound B.
[0073] fixed bed reactor
[0074] Catalyst 1 # ~ Catalyst 5 # After tableting, crushing, and granulation to 0.15mm ~ 0.18mm, they were used for reaction 1 # ~Reaction 5 # . Response 1 # Using a single-tube reactor with an inner diameter of 1 cm, the reaction temperature can be controlled at -30°C through shell-side heat exchange, and the temperature gradient of the catalyst bed in the test is less than 3°C. response 2 # ~Reaction 5 # Using a multi-tubular reactor, the reaction 2 # Two tubular r...
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