HCl Salts and wierd crystals from BF3xEt2O reductions
Hi fellow mad ppl.
SWIIF has been trying to reduce 2,5-dimethoxy-p2np to 2,5-dimethoxy-phenyl-2-isopropyl-hydroxylamine with BF3xEt2O/NaBH4 in THF. Reaction went just as
described in the literature. Then HCl reflux was set up (after quenching with ice), and the solution refluxed for 2 hours. Some white sediments have
collected on the bottom, so ether was added to try and clean it up, but this only promoted the formation of more crystals.
when ether is evaporated the crystals disappear slightly.
up to now 7.7g of clear white crystals have been collected and swiif is waiting for the flask to cool down to collect a second batch.
swiif though is in need of help to identify these xtals. According to shulgin hot compounds (n-hydroxylated) can be made into hcl salt via addition of
concentrated HCl and then addition of ether. In water these crystals do not solublize, but in alcohol (ethanol) they do.
plz advise as to identity of these xtals, as swiif is lost :-|
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