*This article is only used as a laboratory guide for synthesis.
*This article is a guide for the preparation of laboratory chemical raw materials.
*The raw materials and products used in the article are harmful to health. Please handle them with caution.
Improper operation may cause personal injury or even death!
This article mainly introduces the synthesis of ethyl nitrite and how to synthesize azide salts using ethyl nitrite and hydrazine and base.
Synthesis of Ethyl Nitrite
The raw materials required are sodium nitrite and ethanol and water and sulfuric acid.
The addition ratio of raw materials is sodium nitrite:sulfuric acid:ethanol=0.9eq.:0.45eq.:1.eq… At least 100 ml of water is added to each mole of sodium nitrite to dissolve it completely so that a part of ethanol is added later without precipitation. Add 1/3 - 1/4 of ethanol to the sodium nitrite solution to get a liquid, if the a liquid is cloudy, slowly add water to the a liquid until the a liquid is clear; mix the remaining ethanol and sulfuric acid to get b liquid; slowly drop b liquid into a liquid, gas will be produced, which is gaseous ethyl nitrite (pure ethyl nitrite is light yellow in liquid state), export the gas, use -20 ℃ spherical condenser tube for condensation to obtain ethyl nitrite. Nitrogen oxides will be generated if the dropping process is too fast.
Synthesis of Azide Salt
The raw materials required are ethyl nitrite and absolute ethanol and hydrazine hydrate and sodium hydroxide or potassium hydroxide.
The use ratio of the raw materials is ethyl nitrite: hydrazine hydrate: alkali: ethanol = 1 eq.: 1.05-1.1 eq.: 0.9-0.95 eq.: 2-3 eq… Mix pure ethyl acetate, alkali and hydrazine hydrate to form a solution. If the solution is cloudy, you can filter out the solid impurities by suction filtration to obtain a clear liquid. Ethyl nitrite was slowly added dropwise to the mixed solution on a flask in an ice bath with a -20°C condenser, and the temperature in the flask was controlled between 20-35°C. After the dropwise addition, when the temperature begins to drop, remove the ice and stir at room temperature for 1-2h. If the ice will melt completely during the dropping process, please stop the dropping and add ice.
A large amount of powder will gradually precipitate out of the system, which will be pure white finely divided and uniform powder sand-like powder after suction filtration, washing and drying. If the condensation conditions of the system are sufficient, even if the temperature reaches 60 °C for a short time, the intercalation rate and product purity will not be affected very much, but if the condensation conditions are insufficient, it may lead to a large loss of ethyl nitrite.
（Reference has been made to the literature of Japanese chemists, whose work is to add ethyl nitrite, hydrazine, ethanol and alkali into a sealed tube for reaction, and the obtained product can be directly used for synthesis.）
If there is no cold pump to cool the condensing tube, you can also choose to directly pass the generated ethyl nitrite gas into the system slowly, but the temperature control should be more strict, and it should be controlled between 15-25 ℃. A large amount of ethyl nitrate was spilled.
This is a picture of the product