Method for chemically synthesizing 3,5-diio-2-hydroxybenzene formyl chloride

A technology for hydroxybenzoyl chloride and chemical synthesis, which is applied in 3 fields, can solve the problems of high energy consumption in the concentration process, difficult treatment of acidic wastewater, and large hidden dangers in production safety, and achieves low cost, high product yield and purity, and reasonable conditions. Effect

Inactive Publication Date: 2011-10-05
ZHEJIANG RONGYAO CHEM +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Oxalyl chloride is a liquid reagent with high toxicity, strong irritation and strong corrosiveness. It decomposes violently and releases toxic gas when it encounters water. Outstanding environmental problems
The use of thionyl chloride will produce a large amount of asphyxiating sulfur dioxide gas (one of the six indicators strictly controlled by the national environmental protection on the atmosphere), which is difficult to deal with. At present, the mixture of sodium sulfite and sodium chloride is mainly prepared by alkali absorption, and the waste water produced The amount is large, the energy consumption of the concentration process is high, and there are big problems in the market

Method used

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  • Method for chemically synthesizing 3,5-diio-2-hydroxybenzene formyl chloride
  • Method for chemically synthesizing 3,5-diio-2-hydroxybenzene formyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The ratio of the amount of 3,5-diiodo-2-hydroxybenzoic acid and bis(trichloromethyl) carbonate feed material is 1: 0.34, 3,5-diiodo-2-hydroxybenzoic acid and catalyst are 1: 0.01, the catalyst is pyridine, the organic solvent is toluene, and the mass ratio of the organic solvent to 3,5-diiodo-2-hydroxybenzoic acid is 5:1.

[0028] In a 500mL three-necked flask equipped with a thermometer, a reflux condenser and mechanical stirring, add 39.0g (100mmol) of 3,5-diiodo-2-hydroxybenzoic acid and 10.1g (34mmol) of bis(trichloromethyl)carbonate , toluene 224.9mL (195.0g) and pyridine 0.1g (1mmol), warming up to 60 ℃ and stirring reaction for 8h, thin-layer chromatography tracking reaction (developing agent is petroleum ether: ethyl acetate=5: 1 (volume ratio)), the reaction After the end, the reaction solution was evaporated under reduced pressure to remove the solvent, the concentrate was filtered, and dried at 60° C. to obtain 37.5 g of 3,5-diiodo-2-hydroxybenzoyl chloride. ...

Embodiment 2

[0030] 3, the ratio of the amount of 3,5-diiodo-2-hydroxybenzoic acid and two (trichloromethyl) carbonate feed materials is 1: 0.34,3, the ratio of 5-diiodo-2-hydroxybenzoic acid and catalyst feed materials The amount ratio is 1:0.01, the catalyst is N,N-dimethylformamide, the organic solvent is toluene, and the mass ratio of the organic solvent to 3,5-diiodo-2-hydroxybenzoic acid is 10:1.

[0031] In a 1000mL three-neck flask equipped with a thermometer, a reflux condenser and mechanical stirring, add 39.0g (100mmol) of 3,5-diiodo-2-hydroxybenzoic acid and 10.1g (34mmol) of bis(trichloromethyl)carbonate , toluene 449.8mL (389.9g) and N,N-dimethylformamide 0.1g (1mmol), the temperature was raised to 100°C and the reaction was stirred for 8h, and the reaction was tracked by thin-layer chromatography (the developing solvent was petroleum ether: ethyl acetate=5: 1 (volume ratio)), after the reaction finishes, the reaction solution is evaporated under reduced pressure to remove th...

Embodiment 3

[0033]3, the ratio of the amount of 3,5-diiodo-2-hydroxybenzoic acid and bis(trichloromethyl) carbonate feed material is 1:1,3,5-diiodo-2-hydroxybenzoic acid and the ratio of catalyst feed material The amount ratio is 1:0.01, the catalyst is N,N-dimethylacetamide, the organic solvent is toluene, and the mass ratio of the organic solvent to 3,5-diiodo-2-hydroxybenzoic acid is 5:1.

[0034] In a 500mL three-necked flask equipped with a thermometer, a reflux condenser and mechanical stirring, add 39.0g (100mmol) of 3,5-diiodo-2-hydroxybenzoic acid and 29.7g (100mmol) of bis(trichloromethyl)carbonate , toluene 224.9mL (195.0g) and N,N-dimethylacetamide 0.1g (1mmol), warming up to 60°C and stirring for 6h, TLC tracking reaction (developing solvent is petroleum ether: ethyl acetate=5: 1 (volume ratio)), after the reaction finishes, the reaction solution is evaporated under reduced pressure to remove the solvent, the concentrate is filtered, and dried at 60°C to obtain 3,5-diiodo-2-h...

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Abstract

The invention discloses a method for chemically synthesizing 3,5-diio-2-hydroxybenzene formyl chloride. The method comprises the step of: with 3,5-diio-2-hydroxybenzoic acid and di(trichloromethyl) carbonic ester as raw materials, reacting for 1-10 hours at the temperature of 40-150 DEG C in an organic solvent under the action of an organic amine catalyst, and processing reaction liquid to obtain 3,5-diio-2-hydroxybenzene formyl chloride, wherein the charging mol ratio of the 3,5-diio-2-hydroxybenzoic acid to the di(trichloromethyl) carbonic ester is 1: (0.34-2.0), the charging mol ratio of the 3,5-diio-2-hydroxybenzoic acid to the organic amine is 1: (0.01-1.0), and the mass ratio of the organic solvent to the 3,5-diio-2-hydroxybenzene formyl chloride is (5-20): 1. The method disclosed by the invention has the advantages of available raw materials, low cost, simplicity and safety in operation, environmental friendliness and higher product yield and purity and has greater application value and good social and economical benefits.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing an intermediate of iodosamide sodium, in particular to a method for chemically synthesizing 3,5-diiodo-2-hydroxybenzoyl chloride. (2) Background technology [0002] Closantel Sodium (Closantel Sodium) is a broad-spectrum, high-efficiency, low-toxic anthelmintic, which can be used to treat and prevent parasitic infections in cattle and sheep, and can be administered in various forms such as oral or intramuscular injection. The drug is effective against some nematodes and arthropod insects that are in close contact with the blood circulation or blood-sucking parasites, such as adults and larvae of Fasciola hepatica, Fasciola large and Fasciola gigantea, Haemonchus, Sinostomum, Avian mouth nematode, Geiger Nematodes, Chabert's nematodes, etc. have high-efficiency killing effects. Combining with plasma protein in animals, the drug has the effect of prolonging the drug effect, and can prevent cattle an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/05C07C51/60
Inventor 蒋华江洪志陈仁尔苏为科张斌
Owner ZHEJIANG RONGYAO CHEM
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