Question regarding mdp2p Nabh4 reduction

paranoid

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After nabh4 addition is complete and mixed for a few hours after can you let the mix sit for a few hours and the freebase oil layer will rise to the top and can be seperated? this eliminates the need for dcm or toluene extraction but does effect yield.
 

rotovap5002

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Yes it affects yield slightly but it is much faster. Thats how the big labs do it, they skip that step entirely. They just add equal parts water, half cold and half warm.
 

paranoid

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What do you mean add water?
 

Berlin777

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I was told to use 2.7x amount of water, so if RM is 5L it should be 13.5L water, oil is separated and rm is extracted again
 

rotovap5002

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people like using water in excess but in my experience i don't find it necessary. It seperates nicely. I also find that using dcm is not worth the hassle at all.
 

Berlin777

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I also prefer EA instead of DCM, DCM takes ages to spearate
 
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