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Preparation of 3 dodecylsulfonyl propyl 6 tert-butyl 7h[124]triazol[3,4-b][134]thiadiazine

A technology of dodecyl sulfone propyl group and dodecyl sulfone base 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 The effect of low harmful absorption and high coupling activity

Active Publication Date: 2019-02-12
沈阳感光化工研究院有限公司
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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 dodecylsulfonyl propyl 6 tert-butyl 7h[124]triazol[3,4-b][134]thiadiazine
  • Preparation of 3 dodecylsulfonyl propyl 6 tert-butyl 7h[124]triazol[3,4-b][134]thiadiazine
  • Preparation of 3 dodecylsulfonyl propyl 6 tert-butyl 7h[124]triazol[3,4-b][134]thiadiazine

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Embodiment 1

[0026] To the 1000ml there-necked flask equipped with the reflux water separator, add 84g of 4-dodecylsulfonyl butyric acid and 320ml of toluene, be warming up to reflux under stirring, separate the water until the steamed toluene is clarified, be cooled to 60°C and start dripping 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 obtained product was 4-dodecylsulfonyl butyryl chloride. Under reduced pressure distillation (vacuum degree expressed number 0.092MPa) to temperature 55 ℃, stop under reduced pressure distillation and add dry toluene 300ml, cool down to below 25 ℃, add 5-tert-butyl-2-hydrazino-6H-1,3, 61.5 g of 4-thiadiazine hydrochloride was slowly heated to 60-65° C., and the reaction was incubated for 1 hour. Then the temperature was raised to reflux, and the reaction was carried out under reflux for 4 hours. The temperature was lowered to 40° C., 50 ml of 20wt% NaOH aqueous solution...

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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, in particular to 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]-triazole[3,4-b]-[1,3,4]-thiadiazine is An important intermediate of pyrazolotriazole type coupler, this coupler is a new type of magenta coupler that is currently being used in color photographic paper by major film companies at home and abroad. First-generation magenta coupler. [0003] According to relevant literature reports, 3-dodecylsulfonylpropyl-6-tert-butyl-7H-[1,2,4]-triazole[3,4-b]-[1,3,4 The synthetic method of ]-thiadiazine has the following two kinds: [0004] Method 1, the chemical reaction equation is as follows: [0005] [0006] In the method, 4-dodecylsulfonyl butyric acid is used as a raw material, and phosphorus oxychloride is used as a chlorination reagent and a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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