Looked up using NaBH4 and CuCl2, instead of LAH and the paranoia of an incident, and this link is very specific in how it can be used for the 2,5 and the 3,4,5.
- By Rabidreject
That’s strange - did they say they did p2np in a matter of minutes? I’ve been playing with this recently and everytime I just went by colour as a que to add the catalyst I got a really crap yield but when I left it for hours before addding the catalyst the yield was good.
Do you think they are chilling the reaction at first and then bringing up to 80c or are they doing it all at 80c?
Do you think they are chilling the reaction at first and then bringing up to 80c or are they doing it all at 80c?
- By mycelium
I didn't see anything other than the 80c temp. I just re-read it really fast...
There is this, tho....
The application of mild heating is crucial to reach full conversion of the starting materials in the times indicated in Table 1. However, conversion to the desired products is also achievable at room temperature over 18 hour stirring with minor yield loss. Increasing the heating temperature up to 110 °C does not lead to increased product yields
And as far as times go....
Furthermore, studies to identify the highest yielding reaction times (reaction stopped at 10, 15, 30, 45, 60, 75, and 90 minutes) revealed that longer stirring when heating is applied is not beneficial.
The screenshot here shows how long it took to do each of the substances.
There is this, tho....
The application of mild heating is crucial to reach full conversion of the starting materials in the times indicated in Table 1. However, conversion to the desired products is also achievable at room temperature over 18 hour stirring with minor yield loss. Increasing the heating temperature up to 110 °C does not lead to increased product yields
And as far as times go....
Furthermore, studies to identify the highest yielding reaction times (reaction stopped at 10, 15, 30, 45, 60, 75, and 90 minutes) revealed that longer stirring when heating is applied is not beneficial.
The screenshot here shows how long it took to do each of the substances.
Attachments
- By Rabidreject
Yes I did seee this and wondered why he managed to reduce p2np (example 1 in the timings in like 10mins. I am guessing he is doing it all at 80c because I ran this exact reaction a couple of times last week and the first time I used an ice bath, did the addition of p2np over an hour then left it for another 3h in the ice bath, addded the catalyst all at once, heated to 80c for 30mins - yield was great 76% or something.
Then I ran it again a day or so later and I only went by the que of the colour of the RM. Added everything over an hour, then left it one hour (yellow had gone and was white), added the catalyst and heated. Yield was TERRIBLE. I didn’t work out % yield but I ended up with like 1.5-2g of r-amphetamine -from a 10g reduction!
Either way - probably the most relevant and interesting paper I have ever read tbh. A lot of time they are way above my head and only slightly relevant. This was bang on!
Then I ran it again a day or so later and I only went by the que of the colour of the RM. Added everything over an hour, then left it one hour (yellow had gone and was white), added the catalyst and heated. Yield was TERRIBLE. I didn’t work out % yield but I ended up with like 1.5-2g of r-amphetamine -from a 10g reduction!
Either way - probably the most relevant and interesting paper I have ever read tbh. A lot of time they are way above my head and only slightly relevant. This was bang on!
