I wanted to perform a reaction in a sealed tube. My reaction is ester hydrolysis. Since I use less amount of THF as solvent, its hard for me to maintain the reaction condition for long time under reflux condition. Could you please suggest me whether I can perform the reaction in a sealed tube?
Main advantages of reflux (constant temperature environment and mixing with the bubbles) can be implemented on a magnetic stirrer with a temperature controller. It is only necessary to adjust the temperature of the reaction medium so that it was just below (2-3 Celsius grad) of the boiling point. This allow to perform reaction in usual vials and bottles with screw cups, without water reflux condencer. Inert gas (argon, CO2 etc) purging is also good - to avoid slow oxidation of compounds in long-term experiment.
Yes, you can; however, acid hydrolysis is a reversible process. You can use LiOH in a THF-H2O mixture in a sealed tuve (purge oxygen! off)
Usually, ester hydrolysis are pretty easy reaction. I assume your product is quite bulky if you need to heat it up so much. Sealed tube could be one option.
I would suggest to use 1,4-dioxane as a solvent instead of THF with 2M LiOH as the base.
-High boiling solvent (101°C);
-Completely mixes with water - no biphasic mixture or need for methanol as coseolvent;
-Easy work-up (add 3 volume of water and acidify, collect precipitate by filtration).
THF/H2O mixture is good method to have faster hydrolysis and easy too. May be you doing bulk reaction, other wise there is no need for using reflux condition.
Thank you Andrei Rogoza, Teodoro Kaufman, Pierre-André Fournier, Dinesh Bhimareddy and Roila Awang.
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