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Synthetic method of deisopropylaminophosphorus

A technology of propylpamidophos and a synthesis method, which is applied in the field of veterinary drug residue detection and veterinary drug synthesis, can solve problems such as ecological environment toxicity, harm to human health, harm, etc., and achieves easy operation, cost saving, and controllable experimental process. Effect

Inactive Publication Date: 2021-04-13
天津阿尔塔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, in addition to directly endangering human health, veterinary drug residues can also lead to a series of hazards such as microbial resistance and ecological environment toxicity.

Method used

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  • Synthetic method of deisopropylaminophosphorus
  • Synthetic method of deisopropylaminophosphorus
  • Synthetic method of deisopropylaminophosphorus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: the synthesis of intermediate compound (IIa):

[0033]

[0034] Mix the raw material (Ia) (11.6g) with phosphorus trichloride (9.0g), and slowly add triethylamine (6.9g) dropwise under ice-cooling, stir and react for 3.5 hours, add petroleum ether and stir evenly, then carry out vacuum pumping Filtration, the filtrate was concentrated to obtain 20.0g of intermediate (IIa), yield 86.2%.

Embodiment 2

[0035] Embodiment 2: the synthesis of intermediate compound (IIb):

[0036]

[0037] Mix raw material (Ib) (10g) and thion trichloride (8.7g), under ice bath, slowly drop triethylamine (5.2g), stir and react for 5 hours, add petroleum ether and stir evenly, carry out vacuum suction filtration , the filtrate was concentrated to obtain 18.5g of intermediate (IIb), yield 92.0%.

Embodiment 3

[0038] Embodiment 3: the synthesis of intermediate compound (IIIa):

[0039]

[0040] In a 250mL three-necked flask, N 2 Protection, adding intermediate (IIa) (15g), cooling to 0°C in an ice-salt bath, slowly adding methanol (6.0eq, 10.2g) dropwise, then stirring at room temperature for 2 hours, then adding dropwise 70% ethylamine aqueous solution (6.4 g), stirring overnight at room temperature. TLC (PE:EA=10:1) detected that the reaction was complete, the reaction solution was quenched with water, extracted with ethyl acetate, the organic phase was concentrated under reduced pressure, and the crude product was subjected to column chromatography (elution gradient PE:EA=20:1 ) purification to obtain 7.8g intermediate (IIIa), yield 52.0%.

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Abstract

The invention provides a synthetic method of deisopropylaminophosphorus, which belongs to the field of veterinary drug metabolic synthesis. The synthetic method has the advantages of reasonable process design and cheap raw materials, and comprises the following steps: (1) reacting a compound (I) serving as a starting raw material with thiophosphoryl chloride to generate an intermediate compound (II); (2) reacting the intermediate compound II with methanol and ethylamine to generate an intermediate compound (III); and (3) carrying out deprotection on the intermediate (III) to generate a target compound (IV). According to the synthesis method, the target product is obtained through three steps of conventional chemical reactions, the process design is reasonable, the raw materials are cheap, the cost is saved, the experimental process is controllable, the operation is simple and convenient, and the chemical purity reaches 98% or above.

Description

technical field [0001] The invention relates to a method for synthesizing a compound, in particular to a method for synthesizing a metabolite desisopropylbamidophos, which belongs to the field of veterinary drug residue detection and veterinary drug synthesis. Background technique [0002] Residues of veterinary drugs refer to the prototypes of drugs that accumulate or store in cells, tissues or organs after application of veterinary drugs (including drug additives) in food animals, or enter the milk of lactating animals or eggs of laying poultry and their toxicologically significant metabolism. substances and pharmaceutical impurities. At the same time, in addition to directly endangering human health, veterinary drug residues can also lead to a series of hazards such as microbial resistance and ecological environment toxicity. In recent years, with the sharp increase in the types and scope of use of veterinary drugs, coupled with people's increasing concern about food saf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/24
CPCC07F9/2458C07F9/2412
Inventor 张磊刘晓佳韩世磊
Owner 天津阿尔塔科技有限公司