Sciencemadness Discussion Board

LiAlH4 methods questions

marilynv - 27-7-2005 at 15:46

Hi,
I'm trying to do a LiAlH4 hydrenolysis on some sedimentary samples, reducing the sulfoxides to sulfides. I have three issues that I can't resolve through literature sources:
1. Is there any benefit to using dioxane instead of THF as a solvent during reflux?

2. What are the reasons you reflux under argon vs. nitrogen?

3. Since I'm interested in sulfur compounds, I'd rather not do the hydrolysis with sulfuric acid. What are the best alterantives for hydrocarbons and sulfides?

transformer - 28-7-2005 at 03:22

1. dioxane enables a higher reflux temperature

2. argon is heavier then air which effectiveley pushes the air out of the flask

3. aq NaOH and then H2O

[Edited on 28-7-2005 by samsung]