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The thing is, I think I’d rather save my nitroethane for when my 3,4,5-TMOBA comes and I don’t want p2np bad enough to bother obtaining n-butylamine….but iv heard other bulky amine’s work also…would triethylamine work?

This is very useful - I am going to just try to obtain the cyclohexylamine - given how much success I have just had performing the Nitroaldol reaction on 2,5-dmoba - when you actually use the correct catalyst…. iv just performed a couple of reactions using 2,5-dmoba, GAA, ethylenediamine and...

Okay - I have triethylamine?

I FINALLY actually got round to trying this, it’s under reflux now actually - colour is getting there for sure! I *****ing hate the smells you get from putting this rxn together…I really dislike that almonds cherry smell that this aldehyde releases, it’s gross - also is a really heavy liquid...

Oh and as for re-x’ing reagents no matter who they are from…fair play. I shall start doing so in that case… I assume it’s fairly easy - I’ll do it for the next reaction - I have 15g left so can do one more 10g reaction, this time having pre-re-x’d the aldehyde as well. It was a little sandy and...

That’s a really great response to all my ramblings. To be honest iv started working my way through a book called ‘organic chemistry as a second language’ - I know Hamilton Morris recommends it a lot and so far it seems extremely useful but I get the feeling it’s going to take - well, the rest of...

Okay @FENTAMAS, Fair play to you - I at least quadrupled my yield by simply keeping the filtrate and following your instructions. I’m still just filtering the last - I added EVEN more water and got EVEN more precipitation, even when I really was not expecting it and thought the RM was done...

This RXN is the gift that keeps on giving! haha

Ah yes okay - after having re-chilled, 2nd filter, then added water: froze it solid by accident haha brought it back up to 0–2c then re-filtered for a third time. Got a decent amount but most of the ‘goodies’ were stuck (probably when it froze) to the sides and edges of the RB, tried to flush it...

Wow okay, it’s gone like a slushy again after adding water and a while in the freezer - interesting

So do I separate the oil and re-x it from MeOH? Obviously a small amount of it?

Also, I shall dilute it and try it now…. edit: ah interesting - added a load of water to it (cold water from the fridge) and it did basically what happened when I disposed of the last lot but didn’t keep it. Soon as I started pouring in the water, it went from dark red to looking like orange...

lol I did the exact same thing! I’m pretty scared to go near the LAH!

No idea how to upload it to you then….I know there is a way because I simply modified or at least based my spreadsheets on one sent to me for the DMT synthesis, so I know it can be uploaded just don’t know how….maybe in direct messages?….nope thats so odd…if You can help me work out how to...

Okay - as I say, I’m not organised, I’m learning as I go and I take (s)-crappy notes! okay it won’t let me attach either a ‘numbers’ file or an excell file….thats weird…

Oh also 70 because….well that’s what I had in my cupboard and a lot of it -70% iso…as opposed to the 100% stuff iv got. yeah the water thing you mention earlier is what I tried the first time I tried this RXN and didn’t realise I needed GAA. Sorry ‘the water thing’ - not a great description! I...

No I used the same solvent again so 30ml MeOH, I observed it between 5-10 mins for any colour change then pulled it straight off at 10mins. Sorry I didn’t read the IPA numbers too clearly as I didn’t use it….other than using cold IPA to wash stuff out… So this time I set everything up first...

Oh and I have a load of 70% Ipa In the fridge to wash it QUICKLY!

I know you already accounted for excess nitromethane within your numbers so that it goes to completion but last time I thought I would add a tiiiiny bit extra, just in case it was less pure than I figured so I think instead of 4.5g i added 5 or something like I that (I do have it written down...

Okay I tried it again and was strict about the timing and it didn’t crystallise nearly as easily for some reason… Had to really cool it with an ice bath to induce crystallisation this time. I personally think it seemed to work better last time but I guess I can’t say that until iv done a...