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Synthetic method of 2-chloro-4,6-dibutoxypyrimidine

A technology of dibutoxypyrimidine and synthesis method, which is applied in the field of synthesis of 2-chloro-4,6-dibutoxypyrimidine, can solve the problems of easy decomposition and polymerization, unstable temperature, and cannot be industrialized, and achieves easy Recycling, easy recycling, reducing the effect of decomposition

Inactive Publication Date: 2011-12-21
INSIGHT FINECHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Due to problems such as dibutoxymalonimidine hydrochloride and substituted cyanine base and temperature instability, easy decomposition and polymerization, this method currently has the problems of low yield (47%) and high cost, and cannot be industrialized

Method used

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  • Synthetic method of 2-chloro-4,6-dibutoxypyrimidine

Examples

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Embodiment 1

[0034] (1) Synthesis of Dibutoxypropanediamidine Hydrochloride (ADPX01)

[0035] Add 1000ml of ethyl acetate into a 2L four-neck flask, cool down in an ice-salt bath to 0-10°C; pass dry hydrogen chloride gas (292.0g, 8.0mol) for about 60 minutes, add malononitrile (132g, 2.0mol) of butanol (155g, 2.1mol)) solution, after the dropwise addition, keep warm at 10-15°C for 4 hours, filter, and dry the product at 60°C to obtain 406.0g of the product.

[0036] (2) Synthesis of 3-amino-3-butoxy-N-cyano-2-propionamidine (ADPX02)

[0037] Add NaHCO to a 2L four-neck flask 3 (181.0g, 2.2mol) and 1000ml of water, stirred, cooled in an ice-salt bath to below -0°C, added 50% NH 2 CN aqueous solution (214.0g, 2.55mol), add dibutoxypropanediamidine hydrochloride (ADPX01) (406.0g,), monitor the feeding rate through pH, ​​and control the process pH at 9-10; after the reaction, keep warm at about 20°C Suction filtration for 4 hours; the filter cake was rinsed with water, drained and then drie...

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Abstract

The invention relates to a synthesis method of 2-chloro-4,6-dibutoxypyrimidine, which uses malononitrile as a raw material, undergoes reactions such as alcoholysis into salt, cyanamide substitution, chlorination and cyclization, and is synthesized in high yield. With high content of 2-chloro-4,6-dibutoxypyrimidine, all steps have no harsh conditions, simple operation, environmental friendliness, significant social and economic benefits, and are suitable for industrial production.

Description

field of invention [0001] The present invention relates to the synthesis method and production process of 2-chloro-4,6-dibutoxypyrimidine, an important intermediate of medicine and pesticide. , chlorination and cyclization and other reactions to synthesize 2-chloro-4,6-dibutoxypyrimidine, the product purity is greater than 99%, and the total yield is more than 64%. The synthetic method of the present invention has no harsh conditions, simple operation, and environmental protection Friendly, the solvent is easy to recycle and apply, and it is suitable for industrial production. Background of the invention [0002] 2-Chloro-4,6-dibutoxypyrimidine is an important pesticide intermediate. With the in-depth development of pyrimidine pesticides and medicines, 2-chloro-4,6-dibutoxypyrimidine as an intermediate is getting more and more Wide range of applications. Therefore, it is of great significance to develop 2-chloro-4,6-dibutoxypyrimidine. [0003] At present, there are three...

Claims

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Application Information

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IPC IPC(8): C07D239/52
Inventor 凌云吴清来李敬东
Owner INSIGHT FINECHEM
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