Moja sinteza 3-CMC

draconic123

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Zakaj moje olje 3 cmc med kisanjem postane črno? dobim ga točno 5,5-6 in postane črno
 

Jesse_Pinkman_

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Morda prehitro kapnete kislino ... bolje je ohladiti rm in kislino. Ali zakisate organsko plast ali skupaj z vodo?
 
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draconic123

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samo organski sloj, ja, sumim, da prehitro zakisujem.
 

xoxoxoxo

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po dodajanju kisline dobite vidne plasti vode in proste baze?
 

Jesse_Pinkman_

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Če se uporablja dcm, pri uporabi etilacetata vzamete spodnjo/vodno plast
 

Jesse_Pinkman_

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Mislim, da potem delate nekaj narobe... Ali bi radi opisali korake svoje sinteze?
 

draconic123

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Izvedla sem metilaminiranje tako, da sem 2b3c dcm in metilamin pustila 12 ur brez segrevanja samo z mešanjem, odstranila zgornjo plast, 2-krat oprala spodnjo plast, odstranila zgornjo plast, dodala kislino do 6 in tekočina je postala zelo temno rdeča.
 

UWe9o12jkied91d

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Postopek se sliši dobro, kapljajte počasneje z dobrim mešanjem
bodite potrpežljivi tudi s samo DCM, včasih se odloči, da bo izpadel v 2 min, včasih potrebuje eno uro mešanja, aceton bo pomagal tukaj svetujem, da ga uporabite (hladnega, če je mogoče).
 

draconic123

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Pozabil sem tudi omeniti, da sem za kisanje uporabil mešanico 10/100 ml hcl 36 % in acetona. mislim, da je kriv aceton ali pa sem prehitro dodal kislino... ker je imel najprej precej lepo barvo, potem pa je nenadoma postal temen
 

Jesse_Pinkman_

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Ne uporabljam mešanice aceton/hci, samo 37 % iz zamrzovalnika s kapljajočim lijakom, vsake 2-3 sekunde 1 kapljica ... morda enkrat poskusite na ta način
 

Jesse_Pinkman_

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Kot topilo za 2b3c sem uporabil dcm ali etilacetat, poskusil sem oboje s podobnimi rezultati ...
 

draconic123

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Okej, vem, da je neumno, vendar da bo jasno, torej po kisanju vzamete zgornjo ali spodnjo plast za sušenje z uporabo dcm? Sem zmeden.
 
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