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Preparation of 3-dodecylsulfurylpropyl-6-tert-butyl-7H-[1,2,4]-triazol[3, 4-b]-[1,3,4]-thiadiazine

A technology of dodecyl sulfone propyl and dodecyl sulfone butyric acid is applied in the field of pyrazolotriazole product couplers, and can solve the problems of high cost, large environmental pollution, complicated process and the like, and achieves High coupling activity, low harmful absorption effect

Active Publication Date: 2017-07-04
沈阳感光化工研究院有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0011] The object of the present invention is to provide a kind of 3-dodecyl sulfonyl propyl group-6-tert-butyl-7H-[1,2,4]-triazole[3,4-b]-[1,3 , 4]-thiadiazine preparation method, solves the existing problems in the prior art such as complex process, high cost, and relatively large environmental pollution

Method used

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  • Preparation of 3-dodecylsulfurylpropyl-6-tert-butyl-7H-[1,2,4]-triazol[3, 4-b]-[1,3,4]-thiadiazine
  • Preparation of 3-dodecylsulfurylpropyl-6-tert-butyl-7H-[1,2,4]-triazol[3, 4-b]-[1,3,4]-thiadiazine
  • Preparation of 3-dodecylsulfurylpropyl-6-tert-butyl-7H-[1,2,4]-triazol[3, 4-b]-[1,3,4]-thiadiazine

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Embodiment 1

[0026] Add 84g of 4-dodecylsulfonylbutanoic acid and 320ml of toluene to a 1000ml three-necked flask equipped with a reflux water separation device, heat up to reflux with stirring, divide the water until the distilled toluene is clear, cool down to 60°C and start adding dropwise 43.1 g of thionyl chloride was added dropwise in about 30 minutes, then the temperature was raised to 85-95° C. for 2 hours, and the product obtained was 4-dodecylsulfone butyryl chloride. Distill under reduced pressure (vacuum degree indication number 0.092MPa) to a temperature of 55°C, stop the reduced-pressure distillation and add 300ml of dry toluene, lower the temperature to below 25°C, add 5-tert-butyl-2-hydrazino-6H-1,3, 61.5 g of 4-thiadiazine hydrochloride, the temperature was slowly raised to 60-65°C, and the temperature was kept for 1 hour. Then heat up to reflux, reflux for water separation reaction for 4 hours, cool down to 40°C, add 50ml of 20wt% NaOH aqueous solution and stir for 30 min...

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Abstract

The invention relates to the field of pyrazolo-triazole color formers and particularly relates to a method for preparing 3-dodecylsulfurylpropyl-6-tert-butyl-7H-[1,2,4]-triazol[3, 4-b]-[1,3,4]-thiadiazine. According to the method, the target compound is obtained through converting 4-dodecylsulfurylbutyric acid, which serves as a raw material, into 4-dodecylsulfurylbutyryl chloride in a manner of taking thionyl chloride as a chlorating agent, and then, carrying out dehydration and ring closing with 5-tert-butyl-2-hydrazino-6H-1,3,4-thiadiazine hydrochloride. Compared with the traditional pyrazolone color formers, the compound has the advantages of high coupling activity, low harmful absorption and good light, thermal and wet resistance. A dehydrating agent, i.e., phosphorus oxychloride is not used during synthesis, and thionyl chloride can be recovered, so that environmental pollution is greatly improved, and the method can be applied to industrial production.

Description

technical field [0001] The invention relates to the field of pyrazolotriazole couplers, specifically a 3-dodecylsulfonylpropyl-6-tert-butyl-7H-[1,2,4]-triazole[3 ,4-b]-[1,3,4]-thiadiazine preparation method. Background technique [0002] 3-dodecylsulfonylpropyl-6-tert-butyl-7H-[1,2,4]-triazol[3,4-b]-[1,3,4]-thiadiazine is An important intermediate of pyrazolotriazole-type color coupler, which is a new type of magenta coupler currently used by major film companies at home and abroad in color photo paper. A generation of magenta coupler. [0003] According to relevant literature reports, at present, 3-dodecylsulfonylpropyl-6-tert-butyl-7H-[1,2,4]-triazole[3,4-b]-[1,3,4 The synthetic method of ]-thiadiazine has following two kinds: [0004] Method 1, the chemical reaction equation is as follows: [0005] [0006] The method uses 4-dodecyl sulfone butyric acid as a raw material, and uses phosphorus oxychloride as a chlorination reagent and a dehydrating reagent to conver...

Claims

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Application Information

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IPC IPC(8): C07D513/04
CPCC07D513/04
Inventor 刘勇洪柏欣许巍巍刘全群周兆秋
Owner 沈阳感光化工研究院有限公司
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