Method for synthesizing 5-nitro-2-(propylthio) pyrimidine-4, 6-diol through continuous nitration

A technology based on propylsulfide and propylthio, which is applied in the field of continuous nitration synthesis of 5-nitro-2-pyrimidine-4,6-diol, which can solve the problems of excessive local concentration, overheating, explosion, etc., and achieve Effects of avoiding the use of nitric acid, reducing emissions, and reducing safety risks

Active Publication Date: 2021-06-04
山东天铭医药科技有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis of 5-nitro-2-(propylthio)pyrimidine-4,6-diol mainly adopts domestically to dissolve fuming nitric acid in acetic acid, and then add the raw materials to the acid mixture, but the nitration reaction The heat release is very violent, and if there is a little car

Method used

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  • Method for synthesizing 5-nitro-2-(propylthio) pyrimidine-4, 6-diol through continuous nitration
  • Method for synthesizing 5-nitro-2-(propylthio) pyrimidine-4, 6-diol through continuous nitration
  • Method for synthesizing 5-nitro-2-(propylthio) pyrimidine-4, 6-diol through continuous nitration

Examples

Experimental program
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Effect test

Example Embodiment

[0045] Example 1:

[0046] The microchannel reactor was washed with drinking water, and the temperature control device temperature of the reactor was set to 25 ° C, and the ozone cylinder was connected to the microchannel reactor feed port C by the stainless steel pipe. It is weighted 4,6-dihydroxy-2- (propylthio) pyrimidine hydrochloride 10 g (38.6 mmol) to 100 ml of beaker A, and 50 ml of drinking water is added to the beaker A, stirred and dissolved, and spare. 30 ml of 10% sodium hydroxide solution, poured into the beaker D, and the magnetic stirrer was placed in the beaker D and placed on a magnetic stirrer, and the pipe at the discharge port D was attached to the beaker D, spare.

[0047] The feed pump A is opened, and the flow rate of the feed pump A is set to 4 ml / min, and the material in the beaker A is input into the microchannel reactor. After inputting the reactor 8 seconds in the beaker A, the feed pump B is turned on, and the flow rate of the feed pump B is 113 mL ...

Example Embodiment

[0057] Example 2:

[0058] The microchannel reactor was washed with drinking water, and the temperature control device temperature of the reactor was set to 35 ° C, and the ozone cylinder was connected to the microchannel reactor feed port C by stainless steel pipes. It is weighted 4,6-dihydroxy-2- (propylthio) pyrimidine hydrochloride 10 g (38.6 mmol) to 100 ml of beaker A, and 50 ml of drinking water is added to the beaker A, stirred and dissolved, and spare. 30 ml of 10% sodium hydroxide solution, poured into the beaker D, and the magnetic stirrer was placed in the beaker D and placed on a magnetic stirrer, and the pipe at the discharge port D was attached to the beaker D, spare.

[0059] The transfer pump A is opened, and the flow rate of the feed pump A is opened to 8 ml / min, and the material in the beaker A is input in the microchannel reactor. After inputting the reactor 8 seconds in the beaker A, the feed pump B is turned on, and the flow rate of the feed pump B is 226 m...

Example Embodiment

[0061] Example 3:

[0062] The microchannel reactor was cleaned with a drinking water, and the temperature of the reactor was set to 15 ° C, and the ozone cylinder was attached to the microchannel reactor feed port C by stainless steel pipes. It is weighted 4,6-dihydroxy-2- (propylthio) pyrimidine hydrochloride 10 g (38.6 mmol) to 100 ml of beaker A, and 50 ml of drinking water is added to the beaker A, stirred and dissolved, and spare. 30 ml of 10% sodium hydroxide solution, poured into the beaker D, and the magnetic stirrer was placed in the beaker D and placed on a magnetic stirrer, and the pipe at the discharge port D was attached to the beaker D, spare.

[0063] The transfer pump A is opened, and the flow rate of the feed pump A is set to 2 ml / min, and the material in the beaker A is input to the microchannel reactor. After the material in the beaker A, after 8 seconds, the feed pump is turned on, and the flow rate of the feed pump B is 59 ml / min, open the nitrogen dioxid...

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Abstract

The invention discloses a method for synthesizing 5-nitro-2-(propyl thio) pyrimidine-4, 6-diol through continuous nitration. The synthesis method comprises the following steps: in a continuous flow reactor, taking nitrogen dioxide as a main nitrating agent, ozone as an auxiliary nitrating agent and 4, 6-dihydroxy-2-(propylthio) pyrimidine hydrochloride as a main raw material, carrying out nitration reaction to prepare the 5-nitro-2-(propylthio) pyrimidine-4, 6-diol compound. The method is extremely low in EHS risk, simple and convenient to operate, environment-friendly, high in production efficiency, high in yield, high in purity and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry and relates to a method for continuously nitrating and synthesizing 5-nitro-2-(propylthio)pyrimidine-4,6-diol. Background technique [0002] Nitrification is a common organic unit reaction. At present, the widely used nitrating agents include nitric sulfur mixed acid, nitrate ester, metal nitrate and so on. The atomic economy of these processes is not high, and a large amount of waste acid and organic acid wastewater will be generated during the production process, resulting in serious environmental pollution. The nitration reaction exotherms violently. In the case of process deviation (operation failure, cooling failure, temperature control deviation, material ratio deviation, etc.), many nitration impurities and isomerization impurities are likely to be produced, and the reaction safety risk and quality control risk are high. [0003] The preparation of 5-nitro-2-(propylthio)pyrimidi...

Claims

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Application Information

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IPC IPC(8): C07D239/60
CPCC07D239/60
Inventor 李松松孙崇国王显帅宁尚恩邢杨杨
Owner 山东天铭医药科技有限公司
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