4-n-Octadecylphenol synthesis
- Product Name:4-n-Octadecylphenol
- CAS Number:2589-79-9
- Molecular formula:C24H42O
- Molecular Weight:346.59
114235-67-5
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Yield:-
Reaction Conditions:
with sulfuric acid;water;sodium nitrite at 0 - 50;
Steps:
3
In reaction flasks equipped with mechanical stirring and reflux dividers,Added aniline (0.1 mole),N-octadecanol (0.12 mol) and 180 ml of xylene, followed by anhydrous zinc chloride (5 mmol),Heat to 140°C and stir overnight. Detection reaction is complete,After cooling it is used directly in the next reaction.The temperature was lowered to 0° C., and the upper solution was added to 0.14 mol of a 20% aqueous solution of dilute sulfuric acid to control the exothermic temperature of the reaction to not exceed 20° C. The xylene layer was discarded. Dissolve sodium nitrite (0.14 mol) in 250 ml of water and slowly add it dropwise to the above dilute sulfuric acid solution of 4-n-octadecylaniline to control the reaction temperature at 30-50°C. Starch potassium iodide test paper test, when the reaction solution makes starch potassium iodide blue and the color no longer fade, stop dropping. If the amount of sodium nitrite is insufficient, continue dropping until the reaction reaches the end point. Then, the reaction solution was kept stirring at 50° C. until bubbles were no longer generated in the reaction solution, indicating that the hydrolysis process was completed. After thermal stratification, the crude product of the upper layer was subjected to vacuum distillation to obtain 4-n-octadecylphenol, HPLC: 98.4%, and the yield of the two-step reaction was 48%.
References:
CN105016979,2017,B Location in patent:Paragraph 0025-0028
103045-04-1
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