This work has been performed by Mescalito, the Electronic Performer of HyperLab.
Having initially earned his title by offering the ultimate council in the questions concerning electronic devices and other problems of physical nature, this guy later on turned to bee an aspiring, enthusiastic and innovating workbee.
Here’s what his alter ego has done recently (
Post 464442 (missing)
(mescalito: "DOI - óñïåõ!", Russian HyperLab))… the synthesis was carried out after
https://www.thevespiary.org/rhodium/Rhodium/chemistry/doisynth.html
Into a RBF there were placed 60mls 96% EtOH, 700mg 2,5-DMA*1/2H2SO4 and all was mixed until full dissolution. Thence was added 1,46g iodine – and also stirred until all dissolved. Lastly, there was added 1,8g finely ground Ag2SO4. The mixture was stirred for 14hrs at RT, after 2hrs iodine was visibly spent.
The mixtr was filtered, the filter cake washed w/a little EtOH, ethanol fractions pooled and evaporated into the atmosphere on a waterbath. This was mixed with ~30mls water and some (3-4g) alkali. Dark color disappeared and to the surface floated a pinkish-yellow oil, poorly soluble in hexane (as it seems, generally 2,5-diMeO species is poorly soluble in pet ether, but well soluble in C6H6). The oil was extracted 3x10mls and acidified w/HCl. 630mg (61% of theory) of light-pink powder was obtained , mp 200-201 Ñ (lit. 200,5-201,5 - PiHKAL)
Importantly, it should bee noted that this same procedure in hands of Mescalito gave the max. yield of 33% when applied to 2C-H.
Another important point is that under no circumstances a freebase amine should bee used in this reaction. It leads to massive polymerisation, no product possibly isolated.
Antoncho