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Does the synthesis of isopentyl nitrite require a temperature of around 0°C?

2009-02-26View Original

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Isopentyl nitrite is synthesized by adding isopentanol to an aqueous solution of sodium nitrite in the presence of sulfuric acid. Is it necessary to carry out the synthesis reaction at around 0°C, just as with methyl nitrite? What are the problems if it is synthesized at room temperature? Please help and give some advice. Thank you!
Reply #22009-02-26
Dude, you make aphrodisiacs! It has not been done before; there is a literature article you can refer to: Reaction ID 195192, Reactant BRN 1718835 – isopentyl alcohol; Product BRN 969510 – isopentyl nitrite. Number of reaction details: 9. Reaction classification: Preparation. Reagent used: nitrous acid. Temperature: 60 – 70°C. To find similar reactions, click here. Reference 1: 1115086; Journal: Balard; JLACBF; Justus Liebigs Annalen der Chemie; 52; 1844; 313; ISSN: 0075-4617. This post was last edited by shuchang on 2009-2-26 at 15:09
Reply #32009-02-26
It is obtained by the reaction of isopentanol with sodium nitrite. Different operating methods can be used depending on the actual production conditions. 1. The reaction takes place in a synthesis tube; an aqueous solution of sodium nitrite, isopentanol, and hydrochloric acid are respectively fed into the high-level tanks. First, sodium nitrite solution and hydrochloric acid solution are added to the synthesis pipeline at the same rate; once chlorine bubbles appear in the pipeline, isopentanol is slowly added from the top of the pipeline, and the crude product is obtained through synthesis within the pipeline. The final product is obtained through washing, drying, and distillation. 2. The reaction is carried out in a reaction vessel: sodium nitrite, isopentanol, and water are added to the reaction vessel, stirred, and then hydrochloric acid is added dropwise after the temperature is lowered to below 5°C. Keep at 5°C for 1 hour, let it stand, then separate the aqueous layer. Wash the ester layer with water, followed by a wash with sodium carbonate solution, and again with water. After separating the aqueous layer, dehydrate it with anhydrous sodium carbonate and filter. The filtrate is distilled, and the fraction at 97–99°C is collected to obtain isopentyl nitrite.

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