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4,6-dichloropyrimidine production process

A technology of dichloropyrimidine and production process, which is applied in the field of 4,6-dichloropyrimidine production technology, can solve the problems of high cost, cumbersome organic base recovery and reuse process, large amount of catalyst, etc., so as to avoid recovery and reuse , avoid product loss, the effect of high product yield

Inactive Publication Date: 2018-06-19
LIANYUNGANG GUOSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of the above-mentioned shortcoming of the prior art, the object of the present invention is to provide a kind of synthetic method of 4,6-dichloropyrimidine, is used to solve the recovery and reuse process of organic base in the prior art loaded down with trivial details, the consumption of catalyst is big and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 (the contents involved below are all mass contents, DCP is the abbreviation of 4,6-dichloropyrimidine, and DHP is the abbreviation of 4,6-dihydroxypyrimidine)

[0028] In a device equipped with a reflux condenser, a thermometer, a stirrer and a constant-pressure dropping funnel, 4,6-dihydroxypyrimidine (114.3 g, 98% content, 1 mol), phosphorus oxychloride (1140 g, 99%) were added Stir and mix evenly, heat up to 95-100 ° C, and slowly add phosgene (220 g, 99%, 2.2 mol) to react, take samples after 8 hours, and HPLC analysis shows that the content of 4,6-dihydroxypyrimidine is 0.9%, 4,6- The content of dichloropyrimidine was 98.3%, the reaction was completed, and the reaction mixture was rectified under reduced pressure (oil bath temperature 95°C, vacuum degree-0.095MPa) to obtain phosphorus oxychloride 1082g (content 99%); 4,6-dichloropyrimidine 142.8g (content 99.0%), yield 94.9% (calculated as 4,6-dihydroxypyrimidine), wherein W(DCP) refers to the mass of ...

Embodiment 2

[0030] In a device equipped with a reflux condenser, a thermometer, a stirrer and a constant pressure dropping funnel, 4,6-dihydroxypyrimidine (114.3 g, 98% content, 1 mol), phosphorus oxychloride (600 g, 99%) were added And 1000mL of nitrobenzene, stir and mix evenly, heat up to 95-100°C, and slowly add phosgene (220g, 99%, 2.2mol) to react, take samples after 7h, HPLC analysis 4,6-dihydroxypyrimidine content is 0.65 %, the content of 4,6-dichloropyrimidine was 97.8%, the reaction was completed, the reaction mixture was rectified under vacuum (oil bath temperature 95°C, vacuum degree-0.095MPa) to obtain 565g of phosphorus oxychloride (content 99%); 4 , 140.0 g of 6-dichloropyrimidine (content 99.5%), yield 93.5% (calculated as 4,6-dihydroxypyrimidine).

Embodiment 3

[0032]Dissolve 212g triphosgene (99%, 2.1mol) in 500mL nitrobenzene for later use; in a device equipped with a reflux condenser, a thermometer, a stirrer and a constant pressure dropping funnel, add 4,6-dihydroxypyrimidine (114.3g, content 98%, 1mol), phosphorus oxychloride (600g, 99%), stir and mix well, be warming up to 90-95 ℃, add the nitrobenzene solution of triphosgene dropwise, react after sampling for 6 hours and analyze, HPLC analysis showed that the content of 4,6-dihydroxypyrimidine was 0.45%, and the content of 4,6-dichloropyrimidine was 97.1%. After the reaction was completed, the reaction mixture was rectified under reduced pressure (oil bath temperature 95°C, vacuum degree-0.095MPa) to obtain Phosphorus oxychloride 565 g (content 99%); 4,6-dichloropyrimidine 140.8 g (content 99.7%), yield 94.2% (calculated as 4,6-dihydroxypyrimidine).

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Abstract

The invention provides a 4,6-dichloropyrimidine production process which comprises the following steps: 1) mixing 4,6-dyhydroxyl pyrimidine with phosphorus oxychloride, and adding one or a combinationof more of phosgene, diphosgene and triphosgene to implement a reaction; 2) separating and purifying the reaction liquid obtained in the step 1), thereby obtaining phosphorus oxychloride and 4,6-dyhydroxyl pyrimidine, wherein the recycled phosphorus oxychloride is used as a raw material of the step 1) to implement 4,6-dyhydroxyl pyrimidine synthesis reactions. By adopting the process, the tediousprocess of organic alkali recycling and reuse is avoided, no expensive catalyst is used, resource waste and product loss are avoided, the environment can be protected, no extra solid waste is generated, a great amount of phosphorus-containing waste liquids and waste residues are not generated, either, in addition, a high product yield is achieved, good purity is achieved, market sale requirementscan be met without secondary purification, and the process can be applied to large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a production process of 4,6-dichloropyrimidine. Background technique [0002] Pyrimidine compounds have active molecular structures and are intermediates of many medicines and pesticides. Because of their important roles in the field of pesticides and medicines, they have attracted the attention of scholars. When used as a pharmaceutical intermediate, it is mainly used in the production of sulfa drugs, such as sulfamethazine, sulfamethiazole, sulfamotoxine, sulfa-6-methoxypyrimidine, etc.; 4,6-dichloropyrimidine It is also an important intermediate for the synthesis of sulfonamides and fungicides azoxystrobin. [0003] There are many reports in the literature about its preparation method. The most common method is: reacting 4,6-dihydroxypyrimidine with tertiary amines such as triethylamine, pyridine, N,N-dimethylaniline and phosphorus oxychloride at a certain temperat...

Claims

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Application Information

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IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 徐晨朱国庆张鑫周土林
Owner LIANYUNGANG GUOSHENG CHEM
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