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Raw material recovery device and method for preparing acyclovir intermediate diacetylguanine

A diacetylguanine and recovery method technology, which is applied in the field of raw material recovery equipment for the preparation of acyclovir intermediate diacetylguanine, can solve the problems of low yield, achieve high recovery rate, mild conditions, and less waste Effect

Active Publication Date: 2020-11-17
杭州瑞思新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the advantages of low toxicity, low cost and simple operation, but the yield is low, only 60%-75% (Chemical Reagent, 20021: 35-36)

Method used

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  • Raw material recovery device and method for preparing acyclovir intermediate diacetylguanine
  • Raw material recovery device and method for preparing acyclovir intermediate diacetylguanine
  • Raw material recovery device and method for preparing acyclovir intermediate diacetylguanine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The structure of the reaction device is as figure 1. Using vacuum pump 1, a batch of mother liquor of diacetylguanine is transported to reaction kettle 4, and the solvent in the mother liquor is removed by concentration under reduced pressure at 50-100°C. The solvent is cooled to receiving tank 5 through condenser 2, and the waste gas is passed through the waste gas Pipe 13 discharges into the exhaust gas absorption unit. Transfer 250kg of hydrochloric acid (the molar ratio of diacetylguanine to hydrogen chloride is 1:7) and 250kg of water to the reaction kettle 4, and the reaction is complete at 50-100°C. After cooling to room temperature, add 1.88kg of D11 macroporous adsorption Resin (2%, the mass consumption of the adsorbent is 2% of the mass of the material to be recovered), after 2 hours, the feed liquid is separated by the pressure filter 3, and the liquid is transferred to the extraction kettle 6. 94kg of dichloromethane (the mass ratio of the extraction solve...

Embodiment 2

[0043] The structure of the reaction device is as figure 1 , using a vacuum pump 1 to transport a batch of mother liquor of diacetylguanine to the reaction kettle 4, and concentrate under reduced pressure at 50-100°C to remove the solvent in the mother liquor, and the solvent is cooled to the receiving tank 5 through the condenser 2, and the waste gas is passed through The exhaust gas pipe 13 discharges into the exhaust gas absorption device. Transfer 286kg (the molar ratio of diacetylguanine to hydrogen chloride is 1:8) of hydrochloric acid and 286kg of water to the reaction kettle 4 respectively, after the reaction is complete at 50-100°C, after cooling to room temperature, add 2.82kg of D11 macroporous Adsorption resin (the mass consumption of the adsorbent is 3% of the mass of the material to be recovered), the feed liquid is separated by the pressure filter 3 after 2 hours, and the liquid is transferred to the extraction kettle 6. 188kg of toluene (the mass ratio of the ...

Embodiment 3

[0045] The structure of the reaction device is as figure 1 , using a vacuum pump 1 to transport a batch of mother liquor of diacetylguanine to the reaction kettle 4, and concentrate under reduced pressure at 50-100°C to remove the solvent in the mother liquor, and the solvent is cooled to the receiving tank 5 through the condenser 2, and the waste gas is passed through The exhaust gas pipe 13 discharges into the exhaust gas absorption device. Transfer 322kg of hydrochloric acid (the molar ratio of diacetylguanine to hydrogen chloride is 1:9) and 322kg of water to the reaction kettle 4, after the reaction is complete at 50-100°C, after cooling to room temperature, add 4.70kg of D11 macroporous Adsorption resin (the mass consumption of the adsorbent is 5% of the mass of the material to be recovered), the feed liquid is separated by the pressure filter 3 after 2 hours, and the liquid is transferred to the extraction kettle 6. 376kg of ethyl acetate (the mass ratio of the extract...

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Abstract

The invention discloses a raw material recovery device and method for preparing an acyclovir intermediate diacetylguanine. The device comprises a desolventizing, hydrolyzing and adsorbing device, an extracting device, a crystallizing device, a solid-liquid separating device and the like which are connected in sequence. The method comprises the steps of conveying mother liquor of diacetylguanine toa reaction kettle, removing a solvent in the mother liquor through vacuum concentration at the temperature of 50-100 DEG C, cooling the solvent to a receiving tank through a condenser, and other steps. According to the method, impurities in the diacetylguanine mother liquor are hydrolyzed by hydrochloric acid to generate guanine, then macromolecular impurities are adsorbed by macroporous resin, extraction with an organic solvent is performed. and then recrystallization and purification are performed to recover high-purity guanine, thus recycling the compound in the acyclovir intermediate diacetylguanine mother liquor to obtain the acyclovir intermediate. The adopted raw materials and auxiliary materials are cheap, easily available and environment-friendly; equipment requirements are low;operation is simple; condition is mild, three wastes are few, the cost is low, and economic benefit is good, and the method is an environment-friendly process suitable for industrial production.

Description

technical field [0001] The invention discloses a recovery device and method for guanine, in particular, a raw material recovery device and method for preparing acyclovir intermediate diacetylguanine. Background technique [0002] Acyclovir (ACV), whose chemical name is 9-(2-hydroxyethoxymethyl)guanine, can inhibit viral DNA polymerase to block DNA synthesis, and has a strong effect on inhibiting the reproduction of herpes simplex virus It has low cytotoxicity and can be used for herpes simplex virus infection, herpes zoster, Epstein-Barr virus infection and cytomegalovirus infection. In addition, it also has a certain inhibitory effect on hepatitis B virus. The structural formula is as formula (I). [0003] [0004] There are many synthetic processes of acyclovir reported, N 2 , 9-diacetylguanine is an important intermediate in its industrial production, and the current industrial synthesis of N 2 , 9-Diacetylguanine is mainly synthesized by using acetic anhydride as a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/18
CPCC07D473/18
Inventor 颜吉校张治国施旭亮索艳格张富成沈博王佳豪
Owner 杭州瑞思新材料有限公司
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