Chemical Forums
Chemistry Forums for Students => Organic Chemistry Forum => Topic started by: starfish on November 09, 2011, 12:19:58 AM
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Hello,
I am new to this forum. Just to say hi to all of you first.
I got trouble with Raney Ni reduction of nitrile into primary amine. I either have no reaction or reduction to give a mixture of products. since it is my first time to deal with Raney Ni, I wonder I have not captured some tricks in doing such reduction.
The procedure I use is: weigh a slurry of activated Raney Ni in water, wash with methanol for three times, add in my substrate, stir vigorouly, equip with a H2 balloon, fill the flask with H2 gas, and that's it.
Can anyone give some suggestions to me? thank you!
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Hello,
I am new to this forum. Just to say hi to all of you first.
I got trouble with Raney Ni reduction of nitrile into primary amine. I either have no reaction or reduction to give a mixture of products. since it is my first time to deal with Raney Ni, I wonder I have not captured some tricks in doing such reduction.
The procedure I use is: weigh a slurry of activated Raney Ni in water, wash with methanol for three times, add in my substrate, stir vigorouly, equip with a H2 balloon, fill the flask with H2 gas, and that's it.
Can anyone give some suggestions to me? thank you!
Try using a 10% solution of ammonia in methanol. This inhibits the formation of secondary amines.
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I did one years ago with Raney nickel in a Parr apparatus at fairly high pressure. I ran it at the blow out rupture disk pressure, ~1000 psi? The reduction was slow. I don't remember if I heated it too.
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great! Thanks for advices!!! I now just set up a reaction using 2M NH3 in MeOH as solvent. Hope it will work.
:P