This is the result of much effort ,and the information is as accurate as I can remember. I am sure the colors are correct, and that the times, amounts, etc, are reasonably accurate, I didn’t have true scales.<\/p>\n
The amounts<\/b><\/p>\n The DMSO was frozen solid and removed from icebox. Chilled H2SO4 was added to the DMSO chunk. This heats up a little and liquifies, somewhat, the DMSO. Swirl. Add the NaBr and swirl or stir if you have a good enough (BIG) stirbar. Chopping thru the salt is tough.<\/p>\n With vigorous stirring, the dillapiole is dripped into the DMSO\/H2SO4\/NaBr mixture, which btw, is now sodium sulfate, and in situ formed HBr.<\/p>\n The rate is a slow one, taking about an hour to get it all in, keeping it cool in a bath. The mixture , before adding dillapiole, is yellow-orange. The addition of dillapiole decolorizes the mess and then begins a slow progression through the pukey-green, to yellowish, to the legendary burgundy. Really, its just a really dark yellow. Maybe with a orangishness. With proper stirring this takes 24 Hrs. It must always stay cool and stay stirring.<\/p>\n Then add 1L ice-water, decant, and the bromo-dillapiole (a heavy orange syrup) doesn’t need to be distilled, it is good enough for the next stage. The yield was about 70%<\/p>\n Finkelstein Swap<\/b><\/p>\n Measure out an equimolar amount of Sodium iodide, add 5% to that, and suspend your bromo-dillapiole in acetone. Heat it, and as it approaches reflux, carefully add small amounts of the iodide salt to mixture. It darkens, and the reaction is a very visual one, and a very malodourous one, as iodine stinks nicely. Reflux gentle for 30 min (90% yield)!<\/p>\n Delepine reaction<\/b><\/p>\n Put the undistilled iodo-dillapiole in 10x amount of alcohol in a 500ml RB flask, heat and begin adding slight molar excess of hexamine until all is in. Refluxing this for 6 hours gave an eventual yield of DMMDA-2 which is quite rewarding. No one should doubt the power of delepine!<\/p>\n The workup:<\/b><\/p>\n Add HCl until the ph is 2, and filter off the ass-load of formed ammonium chloride<\/p>\n The red liquid is evaporated until a mass of hard rocklike crystals remained. This is impure DMMDA-2. The crystals CANNOT be cleaned, with ether or any other washes. Freebase and distill to give clear, off colored DMMDA-2.<\/p>\n The yield is 50% from the beginning. SWIM got ~12 g at the end.<\/p>\n Delepine Route to DMMDA-2 from Dillapiole By Egotrip This is the result of much effort ,and the information is as accurate as I can remember. I am sure the colors are correct, and that the times, amounts, etc, are reasonably accurate, I didn’t have true scales. The amounts 25 g dillapiole 240 ml DMSO 18g […]<\/p>\n","protected":false},"author":1,"featured_media":1615,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"footnotes":""},"categories":[24],"tags":[],"class_list":["post-918","post","type-post","status-publish","format-standard","has-post-thumbnail","category-quimica-avanzada"],"yoast_head":"\n\n
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