Last these day I have been proving new writeups of amination. Always I have used nitrometane as source of metylamine, with good succes but not perfect results as for yields.
Some time ago I did a few hundreds of grams of metylamine following the bright star´s method that never used. That is to say, with only 1 filtering of the residual ammonium chloride and without doing any type of purification with chloroform or recrystallization.
I am going to prove the variant of reduction with methylamine, methanol,.... proposed by Roundbottom: " Osmium/BrightStar Al/Hg Methylamine Reductive Amination ", posted on Rhodium,since the yields are really interesting, and the process is way more simply and easier than Methyl's man method. I am going to use a scale 10X minor to try with few amounts of ket.
My question is with regard to the quality of the produced methylamine following the bright star´s method:i know that is not pure, something about 95 %, and it must contain significant quantities of ammonium chloride and other amines.. But the production of mda as a side product would not be a problem. Only wish that yields were not lowering in excess due to this lack of purity of the methyilamine.10-20% less hydrocloride would not be a problem to handle.It´s posible to need to add some extra mg. of this methylamine to assure a propper amount of it?
Some experience using methylamine done with this process?
Some time ago I did a few hundreds of grams of metylamine following the bright star´s method that never used. That is to say, with only 1 filtering of the residual ammonium chloride and without doing any type of purification with chloroform or recrystallization.
I am going to prove the variant of reduction with methylamine, methanol,.... proposed by Roundbottom: " Osmium/BrightStar Al/Hg Methylamine Reductive Amination ", posted on Rhodium,since the yields are really interesting, and the process is way more simply and easier than Methyl's man method. I am going to use a scale 10X minor to try with few amounts of ket.
My question is with regard to the quality of the produced methylamine following the bright star´s method:i know that is not pure, something about 95 %, and it must contain significant quantities of ammonium chloride and other amines.. But the production of mda as a side product would not be a problem. Only wish that yields were not lowering in excess due to this lack of purity of the methyilamine.10-20% less hydrocloride would not be a problem to handle.It´s posible to need to add some extra mg. of this methylamine to assure a propper amount of it?
Some experience using methylamine done with this process?