According to this (google cache) the BP of Asarone is 296C.
http://64.233.187.104/search?q=cache:BCx...s&ct=clnk&cd=20
Asarone Isolation from Calamus Roots
The following is a snippet from Uncle Fester's "Practical" LSD Manufacture" But this has nothing to do with LSD production. Enjoy
Calumus oil, if its country of origin is India, consists of about 80% of the allyl isomer of asarone.
Asarone can be purified by distillation under a vacuum to yield fairly pure allyl-asarone. Its boiling point is 296øC at normal pressure and about 170øC with aspirator vacuum. More details on this Indian calamus oil can be found in Chem. Abstracts column 6585 (1935), also Current Science, Volume 3, page 552 (1935).
My search for calamus oil of Indian origin came up empty. In fact, the health-food store in my town, which is well-stocked with various oils for use in aromatherapy, had never heard of the stuff, nor was it listed for sale in their catalogs. This left one alternative: dig up the roots of North American calamus, and steam-distill the oil out of them.
While searching for calamus in my area's swamps, bogs and ponds, the damaging effects of the spread of purple loosestrife was obvious. This imported plant from Europe has taken over much of the former habitat of the calamus plant. Here in America, the loosestrife is free from the insect that keeps it under control in Europe by feeding on its seeds. The state paper-pushers have been thinking for years about importing the bug, without ever getting off their butts and doing it. I suggest this project to somebody out there in the reading public so that it can finally get done while there is still some native flora left.
After a lot of searching, I finally found a large patch of the American calamus. (See Figure 4.)
The time for harvesting the roots of the calamus is in the fall after the killing frost. The frost brings the oil down out of the leaves and into the root for winter storage. The roots are about a foot long, an inch or so in diameter, and run horizontally in the soil at a depth of a few inches. They are best dug out using a fork, taking care not to pierce the root, as this will cause loss of oil during drying. The dug-up roots should be rinsed free of dirt, and the tops cut off there in the field. (See Figure 5.) The roots should then be taken home and allowed to dry at room temperature for a week or two. Take care that they do not get moldy!
Once dried, oil can be distilled from them. This is done by first grinding up the roots in a blender or with a Salad Shooter, and piling the ground-up roots into a large pressure cooker.A good-sized pressure cooker will take a load of 10-15 pounds of root. Next, add a few gallons of water, a couple handfuls of salt, and mix.
The oil can now be distilled. Attach a five-foot length of copper tubing to the steam exit on the lid of the pressure cooker. Its diameter should match that of the steam exit so that steam is not lost here, and should be tightened into place with a pipe clamp. The tubing should then be led downward into a pail of ice water, and back up into a dark-glass 40 or 64 ounce beer bottle. The ice water cools the steam, turning it into water which collects in the bottles.
Heat is applied to the pressure cooker, bringing it to a boil. Heat as fast as is possible without bringing over foam or having uncondensed steam escape. When a couple of gallons have been distilled out, stop the heating and add a couple more gallons of water to the pressure cooker. Continue this process until 4-5 gallons of water have been collected.
This process is a steam distillation, and is the way most plant oils are obtained. The steam distillate in the beer bottles contains calamus oil floating on top of the water and clinging to the glass. Calamus oil produced from American plants is reddish brown, and has a strange, pleasant and sweet odor. For more detailed information on calamus oil see The Chemergic Digest August 30, 1943, pages 138-40, and Soap, Perfumery and Cosmetics August 1939, pages 685-88.
The oil is obtained by first saturating the steam distillate with salt, then extracting the oil with toluene (obtained off the shelf in the hardware store's paint section). About a gallon of toluene is plenty to effect the extraction. Then the toluene is removed by vacuum evaporation in a large filtering flask to yield the calamus oil as a residue in the filtering flask after the toluene has been evaporated. The yield is about 200 ml from 15 pounds of roots.
Calamus oil obtained from sources other than India differs from the Indian oil in two important respects. The amount of asarone in the oil is much lower than the 80% found in the Indian oil, and the position of the double bond is propenyl rather than allyl:
The asarone is obtained in pure form from the oil by fractional distillation under a vacuum. Asarone boils at about 170øC under good aspirator vacuum of 15-20 torr. The asarone fraction should be collected over a 20-degree range centered on 170øC. I found the yield of asarone from American plants to be about 15% of the oil, giving 30 ml from 15 pounds of root.
Asarone is a light-sensitive material, and as such, should be stored in the fridge or freezer. Upon standing in the fridge, it will crystallize, allowing further purification by filtering. The m.p. of the pure substance is 67øC. Asarone is listed as a cancer-suspect chemical, along with half the other substances in the world. In reality it is not particularly harmful. See Chem. Abstracts 1931, page 169. It also doesn't have any pronounced drug effect at reasonable
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