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Author: Subject: Amount of SnCl2 for THF peroxide reduction
tshirtdr1
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[*] posted on 13-12-2014 at 13:17
Amount of SnCl2 for THF peroxide reduction


~5-10 grams? I have some (about a liter of) THF that I hope to use for a grignard reaction. I am trained in computational work, and am new to advanced synthetic techniques. I would like to reduce the peroxides in the THF (will test with KI test before using) with SnCl2, then distill from there to a flask with molecular sieves, with a little mineral oil added in the distillation flask in order to prevent distilling to dryness. The (previously opened) THF has been stored in the dark in a ventilated cabinet for a while, but has probably only been opened once. I appreciate all constructive criticism, but would prefer useful advice. I will be using a fume hood for the distillation.

The reason I chose SnCl2 is because it does not require the addition of water, which will obviously spoil my grignard reaction. I do not plan to use sodium metal, but will use a large quantity of activated sieves to dry a second time. I have argon available, and will store the final dry product under argon. I am trying to both minimize waste and reduce the possibility of explosion. Thanks so much!
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[*] posted on 14-12-2014 at 01:44


It depends how much peroxide you need to destroy. But it sounds like you haven't even tested it for peroxides, so I'm confused as to how you know it contains any peroxide at all.
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tshirtdr1
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[*] posted on 14-12-2014 at 05:16


You're right that I have no idea whether it contains peroxides. I just don't know the scale of reducing agent to add. (milligram or gram) If it is faintly colored, I will add less, and brightly colored, I will add more. I am just assuming the amount is on the gram scale because I correlated it with FeSO4 addition. I guess I will test it and find out myself. Thanks so much!
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