Unlock instant, AI-driven research and patent intelligence for your innovation.
Preparation method of 1-amino-1,2,3-triazole
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of amino and solution, applied in the direction of organic chemistry, can solve the problems of expensive raw materials, unfavorable industrial production, high price, etc.
Active Publication Date: 2021-04-09
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
View PDF3 Cites 0 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
[0012] Different steps of this method use solvents of different polarities, and potassiumpermanganate is used for oxidative cyclization, which will produce solid waste residue, which is easy to generate impurities and is expensive, and this method uses a large amount of methylenechloride, which is highly toxic and the overall preparation The process is cumbersome, the raw materials are expensive, unfriendly to the environment, and not conducive to industrial production
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Image
Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0035] Add hydrazine hydrate N to the 2000mL reaction flask 2 h 4 ·H 2 O (80%) 125.0g (2mol), add glyoxal C dropwise at 0°C 2 h 2 o 2 (40%) 145.1g (1mol), the dropping time is 60min, carries out reduction reaction 2 hours, makes glyoxal dihydrazone solution;
[0036] In the above-mentioned glyoxal dihydrazone solution, pass into ozone (O 3 ) concentration is 127g / m 3 , the aeration time is 240min, and ozone (O 3 ) 62.4g, cyclization reaction at 5°C for 180min to obtain 1-amino-1,2,3-triazole solution;
[0037] The 1-amino-1,2,3-triazole solution was concentrated at 76° C. under a vacuum of 1.03 kPa to obtain 58.80 g of the product, with a yield of 70% and a purity of 99.3%.
Embodiment 2
[0039] Add hydrazine hydrate N to the 2000mL reaction flask 2 h 4 ·H 2 O (80%) 187.5g (3mol), 0 ℃ drop glyoxal C 2 h 2 o 2 (40%) 217.65g (1.5mol), the dropping time is 120min, carries out reduction reaction 3 hours, makes glyoxal dihydrazone solution;
[0040] In the above-mentioned glyoxal dihydrazone solution, pass into ozone (O 3 ) concentration is 130g / m 3 , the aeration time is 360min, and ozone (O 3 ) 100.8g, cyclization reaction at 45°C for 120min to prepare 1-amino-1,2,3-triazole solution;
[0041] The 1-amino-1,2,3-triazole solution was concentrated at 78°C under a vacuum of 1.03kPa to obtain 90.72g of the product, with a yield of 72% and a purity of 99.4%.
Embodiment 3
[0043] Add hydrazine hydrate N to the 2000mL reaction flask 2 h 4 ·H 2 O (80%) 162.5g (2.6mol), add glyoxal C dropwise at 0°C 2 h 2 o 2 (40%) 188.5g (1.3mol), dropwise time is 170min, carries out reduction reaction 1 hour, makes glyoxal dihydrazone solution;
[0044] In the above-mentioned glyoxal dihydrazone solution, pass into ozone (O 3 ) concentration is 129g / m 3 , the aeration time is 340min, and ozone (O 3 ) 93.6g, cyclization reaction at 25°C for 180min to prepare 1-amino-1,2,3-triazole solution;
[0045] The 1-amino-1,2,3-triazole solution was concentrated at 80° C. under a vacuum of 1.03 kPa to obtain 81.90 g of the product, with a yield of 75% and a purity of 99.3%.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
PUM
Login to View More
Abstract
The invention relates to a preparation method of 1-amino-1,2,3-triazole, and belongs to the technical field of medicine synthesis. The preparation method comprises the following steps: (1) adding glyoxal into hydrazine hydrate, and carrying out reduction reaction to prepare a glyoxal dihydrazone solution; (2) introducing ozone into the glyoxal dihydrazone solution, and carrying out cyclization reaction to obtain a 1-amino-1,2,3-triazole solution; and (3) concentrating and filtering to obtain a 1-amino-1,2,3-triazolesolid. According to the method, a one-pot method is adopted, ozone is selected as an oxidation cyclization catalyst, water is selected as a solvent, solvent replacement and addition are not needed in the whole process, use of toxic initial reactants is avoided, and no solid waste is generated.
Description
Technical field [0001] The invention relates to a preparation method of 1-amino-1,2,3-triazole and belongs to the technical field of pharmaceutical synthesis. Background technique [0002] 1-Amino-1,2,3-triazole (C 2 H 4 N 4 ) is an important organic synthesis intermediate that can be used to synthesize a variety of complex compounds in the fields of drugs, fungicides and other fields. For example, it is one of the key intermediates in the synthesis of tazobactam. [0003] At present, the synthesis routes of 1-amino-1,2,3-triazole mainly include the following: [0004] (1) Chinese patent CN 1136809A discloses the reaction of glyoxal and hydrazine hydrate in water to generate intermediate 1, evaporating the solvent under reduced pressure, extracting with ethyl acetate, evaporating the solvent, and then adding a transition metal with water as the solvent. The oxide and hydrogenperoxide are reacted, insoluble substances are removed by filtration, and the solvent is distill...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to View More 
Login to View More