The Hive > Methods Discourse
another question
indole_amine:
...what about this?
"Anyway, when the water had been removed via dean-stark, SWIA distilled away the toluene (still using the trap), refilled the trap with water to the top and during the next 4 hours slowly removed the water in increments of 4-5 drops a time. Temp. climbed to 180°C, where it was held for 1h. On cooling, nothing solidified.."
and
"The reason for the additional solvent was the small amount of starting material"
Post 517101 (missing) (armageddon: "92% is no myth", Methods Discourse)
And although I doubt that Armageddon used >98% pure ketone from "official sources" ;) , I remember that he distilled his ketone at least twice, and also purified it via oxime recrystallization (or was it bisulfite?) - so the purity should've been quite good...
indole_amine
LaBTop:
Post 517198 (missing) (Rhodium: "Quality control of provided data points", Methods Discourse)
And ofcourse the method SWIA used is totally different from the one Zealot proposed.
A really convincing check of the proposed method should be performed with 1 gmol P2P.
And I would like to sea someone try the Raney nickle patent. And report back. LT/
indole_amine:
I think Rhodiums answer was dedicated to Armageddon, not me...
And, by the way:
"although he tried it numerous times, with highest purity reagents, exactly same amounts, appropriately sized glassware and the utmost care to do good lab work - 55% yield!"
Post 528023 (armageddon: "92% are impossible to achieve..", Methods Discourse)
The road is open for new explorers in this field! ;)
indole_amine
LaBTop:
is of the utmost importance, and I highly appreciate your remarks, showing us that at least he tried everything he could to obtain the advertized yields. And that's the most important part of this board, those who dare to investigate, and try to copy referenced procedures in a homebrew fashion.
If we all had sophisticated labs to experiment in, we all would move to purely scientific forums or journals.
And this board would die.
Since it is the research of -many- members which will definitely proof that a proposed procedure can not or can be duplicated, we need more input from others to lay this discussion to rest.
I would like to hear from Antoncho, if he could get in contact with Zealot again, for his view on Armageddons results.
And if their ever was a discussion in the russian forum on this subject, and what their verdict was.
LT/
Smilaxium:
The authors claim to have 80% of analyticaly pure alpha-methylbenzylamine when reacting acetophenone with plain formamide and water for 6 hours at 180 C, followed by an HCL hydrolysis. Would this work for P2P ?
Carlson et. al, Acta Chemica Scandinavia, 1993, 47, 1046-1049
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