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A kind of preparation method of 2,4-dichloropyrimidine and its derivatives

A technology of dichloropyrimidine and its derivatives, which is applied in the field of preparation of 2,4-dichloropyrimidine and its derivatives, can solve the problems of large phosphorus-containing wastewater discharge and unfriendly environment, and achieve large discharge and reduce environmental pollution Problems, the effect of high conversion rate of finished products

Active Publication Date: 2020-12-08
杭州布朗生物医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The invention provides a preparation method of 2,4-dichloropyrimidine and its derivatives, which solves the problems of large phosphorus-containing wastewater discharge and unfriendly environment in the traditional process

Method used

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  • A kind of preparation method of 2,4-dichloropyrimidine and its derivatives
  • A kind of preparation method of 2,4-dichloropyrimidine and its derivatives
  • A kind of preparation method of 2,4-dichloropyrimidine and its derivatives

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preparation example Construction

[0025]A method for preparing 2,4-dichloropyrimidine and its derivatives, comprising a catalyst, compound 1 and phosgene, in the solvent, the compound 1 is reacted with phosgene under the action of the catalyst;

[0026]The reaction of the compound 1 on the catalyst is as follows:

[0027]

[0028]X is any one of H, Cl, Br;

[0029]The structure of the catalyst is as follows:

[0030]

[0031]R1 is C1-10, R2=C1-10, R3=C1-10, R1, R2, R3 are the same, preferably R3PO compounds, where R=C1-10 alkyl or phenyl, preferably triphenylphosphine oxide , Tributyl phosphine oxide and trioctyl phosphine oxide, the catalyst can be reused.

[0032]Which includes the following steps:

[0033]Step 1: Take compound 1, catalyst and solvent into a three-necked flask with a thermometer, agitator, gas tube, and condenser (-5 to -10°C) to prepare the mixture, and use nitrogen to check for leaks;

[0034]Step 2: Heat the mixture prepared in step 1 to 20°C to 90°C, and pass the phosgene under the reaction liquid surface through the ga...

Embodiment 1

[0044]Uracil (51.8 g, 98% content; 0.45 mol), triphenylphosphine oxide (31.3 g, 98% content; 0.11 mol), and nitrobenzene (100 ml) are packed in 250 ml with a thermometer In a three-necked flask with stirring, gas pipe and condenser (-5—-10℃), the system uses nitrogen to check for leaks. The uracil mixture was heated to 60°C, and phosgene (180 g, 99% content; 1.8 mol) was passed through the airway to the reaction liquid surface. During the addition, a small amount of phosgene began to reflux. The phosgene penetration time is 20 minutes. The mixture was heated to 105°C. When the temperature is 90°C, a large amount of gas is released, and a large amount of phosgene in the condenser is refluxed. After 20 minutes, the reaction mixture was clear red. The gassing rate after 40 minutes was very slow; the reaction solution was sampled and the reaction was continued for 1 hour, during which all gassing had ceased. HPLC analysis indicated that the reaction was complete. The reaction mixture wa...

Embodiment 2

[0047]5-Bromouracil (191 g, 99.5% content; 1 mol), tributyl phosphine oxide (111.2 g, 98% content; 0.5 mol) and butyronitrile (200 ml) are packed into 1000 ml tape In a three-necked flask with thermometer, stirring, constant pressure funnel, and condenser (-5 to -10°C), the system uses nitrogen to check for leaks. The 5-bromouracil mixture was heated to 80°C, and solid phosgene (320 g, 99% content; that is, 3.2 moles) and 400 ml of butyronitrile solution were added dropwise to the reaction solution via a constant pressure funnel. During the dropping process, a small amount of phosgene began to reflux. The phosgene addition time is 70 minutes. The mixture was heated to 125°C. When the temperature is 90°C, a large amount of gas is released, and a large amount of phosgene in the condenser is refluxed. After 40 minutes, the reaction mixture was clear red. The gassing rate after 40 minutes was very slow; the reaction solution was sampled and the reaction was continued for 1 hour, during ...

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Abstract

The invention discloses a preparation method for 2,4-dichloropyrimidine and derivatives thereof. A catalyst, a compound 1 and phosgene are involved in the preparation method. The compound 1 reacts with the phosgene under the action of the catalyst in a solvent. The preparation method is reasonably designed, is convenient for use and is capable of solving the problems of high discharge of phosphorus wastewater and environmental pollution of the traditional process; the end product prepared according to the method is high in conversion rate, the preparation period is short and the problem of environmental pollution is reduced; the method is energy-saving and environment-friendly and is suitable for extensive promotion.

Description

Technical field[0001]The present invention relates to the technical field of 2,4-dichloropyrimidine and its derivatives, in particular to a method for preparing 2,4-dichloropyrimidine and its derivatives.Background technique[0002]Pyrimidine compounds are important living substances, which are widely present in organisms and have strong biological activity and have received widespread attention. 2,4-Dichloropyrimidine and its analogues are a kind of pharmaceutical intermediates and reactive dye intermediates. As the demand for end products increases, the demand for such intermediates continues to increase. Therefore, it is particularly important to study its synthesis and develop a green and environmentally friendly process suitable for mass production needs. At present, domestic and foreign companies adopt the phosphorus oxychloride method with traditional processes, which causes great environmental pollution.Summary of the invention[0003]The invention provides a preparation method ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 黄国祥马肖克
Owner 杭州布朗生物医药科技有限公司
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