Preparation method of 1H-1, 2, 3-triazole
A technology of triazole and 1H-1, which is applied in the field of preparation of 1H-1,2,3-triazole, can solve the problems of low production efficiency, production safety risks and the like, and achieves short production route and high atom utilization rate. , The effect of route economy and environmental protection
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Embodiment 1
[0043] Dissolve 80.0g of sodium nitrite (MW69.00, 1.16mol) in 250g of purified water, stir and dissolve at 30-40°C, then cool to 0-5°C to obtain an aqueous solution of sodium nitrite for use.
[0044] Add 94.5g of 1,2-diaminoethylene hydrochloride (1.00mol) into 250g of glacial acetic acid, stir to dissolve and clarify, cool down to -10~0°C, and add dropwise 330.0g of sodium nitrite solution prepared in advance , temperature control -5 ~ 5 ℃. After dropping, continue to stir and react at 0-5°C for 20 minutes, then slowly raise the temperature to 70-80°C, and keep the reaction for 1 hour.
[0045] After the reaction, concentrate under reduced pressure to recover acetic acid, then cool to 0-5°C, adjust the pH to 8-9 with 10% lye (sodium carbonate aqueous solution), then extract with 800mL dichloromethane several times, and combine the organic layers , concentrated to obtain 68g triazole crude oil.
[0046] Then transfer 68g of triazole crude oil into a 100mL roundness rectific...
Embodiment 2
[0050] Add 94.5g of 1,2-diaminoethylene hydrochloride (1.00mol) into a mixture of 100g of water and 300g of glacial acetic acid, stir to dissolve, cool down to -10~-5°C, and add in batches 85.0g sodium nitrite (MW69.00, 1.23mol), temperature control -10~0℃. After the addition is complete, continue to stir and react at -10 to -5°C for 30 minutes, then slowly raise the temperature to 40 to 50°C, and keep the reaction for 2 hours.
[0051] After the reaction is over, concentrate under reduced pressure to recover acetic acid, add 100g of water, adjust the pH to 9-10 with 10% lye, extract with 1000mL of ethyl acetate, combine the organic layers, and concentrate to obtain 69.5g of triazole crude oil .
[0052] Then transfer 69.5g of triazole crude oil into a 100mL roundness rectification flask, carry out high vacuum column rectification, collect 90~95°C fractions (absolute pressure≤5mmHg), and obtain 64.5g of colorless and transparent liquid 1H-1 , 2,3-triazole, the purity is grea...
Embodiment 3
[0054] After mixing 200g of water and 200g of glacial acetic acid, add 85.0g of sodium nitrite (MW69.00, 1.23mol) under stirring, and after dissolving and clarifying, cool to -10~-5°C. Then, 94.5 g of 1,2-diaminoethylene hydrochloride (1.00 mol) was added to the above reaction solution in small amounts and in batches, the temperature was controlled at 0-5° C., and the addition time was controlled at 0.5-1.0 h. After the addition is complete, continue to stir and react at 0-5°C for 15 minutes, then slowly raise the temperature to 50-60°C, and keep the reaction for 2 hours.
[0055] After the reaction was finished, concentrate under reduced pressure to recover acetic acid, adjust the pH to 9-10 with 10% lye, extract with 1000 mL of dichloromethane in portions, combine the organic layers, and concentrate to obtain 69.0 g of triazole crude oil.
[0056] Then transfer 69.0g of triazole crude oil into a 100mL roundness rectification flask, carry out high vacuum column rectification,...
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