Method for preparing 5-fluorocytosine using microchannel reactor
A microchannel reactor, flucytosine technology, applied in the field of preparation of 5-fluorocytosine, can solve the problems of low conversion rate of raw materials, poor product selectivity, long reaction time, etc., and achieves good product selectivity and short residence time. , good mixing effect
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Embodiment 1
[0037] like figure 1 As shown, using Dow Corning's G1 SiC Reactor reaction equipment, using a metering pump to pump cytosine formic acid solution (10wt%) and fluorine gas (mixed in nitrogen, volume concentration 10vol%) into the mixer of the microchannel reactor at the same time , the microchannel reactor has the straight-through channel of tubular structure, and the enhanced mixing channel with T-shaped structure, controls cytosine solution (10wt% formic acid solution) flow rate 580g / h, fluorine gas (mixed in nitrogen, volume concentration 10vol %) The flow rate is 200g / h, and the reaction is carried out at 9°C in a controlled microchannel thermostatic reactor, and the residence time of the reaction solution is 300s. A product solution containing 5-fluorocytosine product was obtained. Add 500ml of n-butanol therein, separate out white product, filter and dry to obtain product 5-fluorocytosine, product detects through liquid chromatography HPLC, the result is: 5-fluorocytosin...
Embodiment 2
[0039]Using the G1 SiC Reactor reaction equipment of Dow Corning Company, the cytosine formic acid solution (10wt%) and fluorine gas (mixed in nitrogen, volume concentration 10vol%) were simultaneously pumped into the mixer of the microchannel reactor using a metering pump. The reactor has a straight-through channel with a tubular structure and an enhanced mixing channel with a T-shaped structure, controlling the flow rate of cytosine solution (10wt% formic acid solution) to 550g / h, and the flow rate of fluorine gas (mixed in nitrogen, volume concentration 10vol%) The temperature is 180g / h, and the reaction is carried out at 5°C in a controlled microchannel thermostatic reactor, and the residence time of the reaction liquid is 240s. A product solution containing 5-fluorocytosine product was obtained. Add 500ml of n-butanol therein, separate out white product, filter and dry to obtain product 5-fluorocytosine, product detects through liquid chromatography HPLC, the result is: 5...
Embodiment 3
[0041] Using the G1 SiC Reactor reaction equipment of Dow Corning Company, the cytosine formic acid solution (10wt%) and fluorine gas (mixed in nitrogen, volume concentration 20vol%) were simultaneously pumped into the mixer of the microchannel reactor using a metering pump. The reactor has a straight-through channel with a tubular structure and an enhanced mixing channel with a T-shaped structure, controlling the flow rate of cytosine solution (10wt% formic acid solution) to 580g / h, and the flow rate of fluorine gas (mixed in nitrogen, volume concentration 10vol%) The temperature is 150g / h, and the reaction is carried out at 10°C in a controlled microchannel constant temperature reactor, and the residence time of the reaction liquid is 60s. A product solution containing 5-fluorocytosine product was obtained. Add 500ml of n-butanol therein, separate out white product, filter and dry to obtain product 5-fluorocytosine, product is detected by liquid chromatography HPLC, the resu...
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