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taffy
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Registered: 2-1-2014
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100g tech. grade adipic acid was agitated in a 250ml RB flask in an aluminum foil bath with 10g tech. 99% calcium hydroxide for several minutes and
then dry distilled for several hours until the still head temp. had began began to stabilize at approx. 160C. After the temp began to drop below 100C
and the distillation appeared to stop the heating was ceased.
The distillate consisted of a biphasic liquid: a pale yellow transparent peppermint-scented upper phase, and a small aq. phase. The distillate was
treated with a small amount of saturated aq. K2CO3, and the organic phase seperated. This was repeated until CO2 evolution had ceased. The crude
ketone was dried over K2CO3, and then redistilled collecting the fraction at approx. 130C. Yield: 28g ketone.
...I believe the remaining large rock of solids in the distilling flask can be further distilled (most of the flask volume appeared to be only
slightly decreased). I think I stopped too early. In any case, I'll report back if any further ketone can be recovered.
[Edited on 10-3-2015 by taffy]
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NexusDNA
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What is the use of cyclopentanone? Nice smell?
Would poly(valerolactone) be nice for demonstration purposes on video? δ-valerolactone could be made from cyclopentanone with a Reimer-Tiemann
reaction.
[Complementing question]
[Edited on 15-3-2015 by NexusDNA]
Bromine, definitely bromine.
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taffy
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In regards to my previous post, no further ketone could be recovered from the boiling flask and the final yield after a redistillation of the
distillate was 28g(bp. ~130C) of a clear, transparent peppermint scented liquid...slightly sol. in water.
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