I recently run into a Methylamine 40% solution supply problem so i went down the HCL route to continue production.
I searched everywhere on here and the web to find instructions on how to use M HCL instead of M40% for reaction.
After many many failed or very poor yeild attepts with info found mostly on here and reddit i have found the a method thats works for me perfectly.
Im no Chemistry expert at all but as Einstein himself said "Insanity is doing the same thing over and over and expecting different results"
Here is my formula for using Methylamine HCL to replace the 40% soloution
>40g M-HCL in 100ml water (Deionized)
>17g NaOH in 50ml wather (Deionized)
>Add all M-HCL slowly to mix, shortly after slowly add the NaOH mix until PH12 is reached
>Continue as normal as if M40% had been added
What i found was the instructions and advice in other posts way over shoot the NaOH alkaline soloution that releases the Methylamine gas from the HCL.
As soon as i held back on adding large quantities of the NaOH soloution i started getting much better yields.
After so many failed attempts following advice i read i decided to monitor the PH through the whole process and found that when adding so much NaOH made the PH alkaline way off the PH scale.
I slowly added small amounts of NaOH solutuin until the reaction mix reached around PH12
At PH12 it was clear that the mix was producing gasses with the way it reacted with the litmus paper
My opinion is that the mix was alkaline and burning the product, please remember im not in anyway an expert on any of this chemistry stuff and found a way it works for me.
Also i used Toluene or Xylene to dissolve and extract
DMSO was used in my reaction instead of NMP
I hope this can method can work for someone else having problems with using Methylamine HCL for reaction
I searched everywhere on here and the web to find instructions on how to use M HCL instead of M40% for reaction.
After many many failed or very poor yeild attepts with info found mostly on here and reddit i have found the a method thats works for me perfectly.
Im no Chemistry expert at all but as Einstein himself said "Insanity is doing the same thing over and over and expecting different results"
Here is my formula for using Methylamine HCL to replace the 40% soloution
>40g M-HCL in 100ml water (Deionized)
>17g NaOH in 50ml wather (Deionized)
>Add all M-HCL slowly to mix, shortly after slowly add the NaOH mix until PH12 is reached
>Continue as normal as if M40% had been added
What i found was the instructions and advice in other posts way over shoot the NaOH alkaline soloution that releases the Methylamine gas from the HCL.
As soon as i held back on adding large quantities of the NaOH soloution i started getting much better yields.
After so many failed attempts following advice i read i decided to monitor the PH through the whole process and found that when adding so much NaOH made the PH alkaline way off the PH scale.
I slowly added small amounts of NaOH solutuin until the reaction mix reached around PH12
At PH12 it was clear that the mix was producing gasses with the way it reacted with the litmus paper
My opinion is that the mix was alkaline and burning the product, please remember im not in anyway an expert on any of this chemistry stuff and found a way it works for me.
Also i used Toluene or Xylene to dissolve and extract
DMSO was used in my reaction instead of NMP
I hope this can method can work for someone else having problems with using Methylamine HCL for reaction
