Method of preparing isoquinine ring compound by adopting micro-channel modular reaction device
The invention discloses a method of preparing an isoquinine ring compound by adopting a micro-channel modular reaction device. The method comprises the following steps of: respectively injecting alcohol liquor of aromatic aldehyde and alcohol liquor of aromatic amine into a first micro-channel modular reaction device by two constant-flow pumps and reacting at a temperature of 85 DEG C-125 DEG C under normal pressure, wherein retention time is 3 minutes-7 minutes; respectively injecting mixed alcohol liquor of cyclohexenone and phosphotungstic acid into a second micro-channel modular reaction device by discharging of the constant-flow pumps and the first micro-channel modular reaction device, and reacting at the temperature of 100 DEG C-140 DEG C under the normal pressure, wherein the retention time is 10 minutes-25 minutes; guiding products into a separator, stewing and layering, and getting supernatant liquid to obtain the isoquinine ring compound. The preparation method of the isoquinine ring compound provided by the invention is a continuous process; moreover, preparation process is simple and easy to operate and control, safety is high, process flow is shortened, production cost is lowered, content of byproducts is lowered, product quality is stable and conversation rate is high. 1. A modular reaction device adopts the micro-channel of the method for preparing the compound of preparation Isoquinuclidine, characterized in that the aromatic aldehyde and ethanol solution of ethanol solution of the aromatic amine, respectively through two constant flow pump is injected into the 1st modular reaction device in the micro channel, and the atmospheric pressure the 85-125 react under [...] , dwell time 3-7min; cyclohexenone and phosphotungstic acid mixed ethanol solution through the constant flow pump and micro channel 1st modular reaction device discharging respectively injected into a 2nd modular reaction device in the micro channel, and the atmospheric pressure the 100-140 react under [...] , dwell time is 10-25min, the product is introduced into the separator, static hierarchical, heating the upper layer of liquid, to obtain. 2. Micronisers channel modular reaction device for the method for preparing the compound of preparation Isoquinuclidine according to Claim 1, characterized in that the stated Isoquinuclidine compounds are of formula I compound shows , aromatic c a compound represented by the general formula II, aromatic amine compound represented by the general formula III: wherein R1 and R2 are independently hydrogen, alkyl, alkoxy, halogen, nitro or cyano. 3. Micronisers channel modular reaction device for the method for preparing the compound of preparation Isoquinuclidine according to Claim 2, characterized in that the stated R1 is hydrogen, methyl, methoxy, fluoro, chloro, bromo, nitro or cyano, the R2 is hydrogen, methyl, methoxy, chloro, bromo or nitro. 4. Micronisers channel modular reaction device for the method for preparing the compound of preparation Isoquinuclidine according to Claim 1, characterized in that the ethanol by acetonitrile, tetrahydrofuran, chloroform, diethyl ether or toluene replacement. 5. Micronisers channel modular reaction device for the method for preparing the compound of preparation Isoquinuclidine according to Claim 1, characterized in that the aromatic aldehyde molar ratio of the aromatic amine 1:1-2. 6. Micronisers channel modular reaction device for the method for preparing the compound of preparation Isoquinuclidine according to Claim 1, characterized in that with cyclohexene molar ratio of aromatic aldehydes 2-10:1. 7. Micronisers channel modular reaction device for the method for preparing the compound of preparation Isoquinuclidine according to Claim 1, characterized in that the quality of phosphotungstic acid of the cyclohexenone the amount of 1%-10%. 8. Micronisers channel modular reaction device for the method for preparing the compound of preparation Isoquinuclidine according to Claim 1, characterized in that the micro-channel 1st modular reaction device comprises of which are connected in sequence through a pipeline 1st micro mixer, micro-structure 1st heat exchanger, the temperature control module and a tubular 1st 1st micro-structured reactor; the 2nd modular reaction device comprises a micro-channel which are connected in sequence through a pipeline of the micro-mixer 2nd, 2nd micro-structure heat exchanger, the temperature control module and a tubular 2nd 2nd micro-structured reactor.