Sinteza P2P iz glikidatnih etrov BMK

blackburn

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kako pride do tega, da po hidrolizi s HCI v dobimo bistro rumeno/temno olje na vrhu tekočine.

po ločitvi olja od HCI in izpiranju z vrelo vodo pa se olje zelo gosto usede na dno in postane motno skoraj kot med.
WUdareFDp4
WB9Kadtprh
 
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w2x3f5

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Njegov glicidat samo brez natrija, standardna težava in običajno se zgodi, ker HCl ni tako dobro delo
 
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G.Patton

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Pozdravljeni, verjetno je vaša težava v parni destilaciji?
 

G.Patton

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Izgleda, da ni dobro ločena rešitev.

P.S. lahko me vprašate v DM. I če brezplačno. Ni vam treba plačati. :)
 

blackburn

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Tako zdaj poskusimo s fosforjem 85%

Imamo enak rezultat, dobro olje po 5 urah refluksa , vendar vzamemo nekaj vzorca in ga speremo z vročo vodo, olje pa se spusti na dno in postane malo lažje, preverite sliko na desni strani. @G.Patton @Ra226

5ysQYZi0kA
 
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blackburn

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9WwHAx1c8X
 
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w2x3f5

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Danes sem od drugega uporabnika prejel kratko poročilo o hidrolizi natrijevega glicidata. Preizkusil je dve moji možnosti, v prvem primeru je iz 20 gramov glicidata prejel 9,2 ml p2p (po odcejanju 8 ml, morda je del p2p izgubil na sušilnikih), pri drugi različici hidrolize pa je iz 20 gramov prejel 12 ml p2p (ni znano, ali gre za suh p2p ali ne ). Teoretični reakcijski donos je 13,5 ml p2p ketona
 

G.Patton

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Ali ste prepričani, da imate točno BMK glicidat?
 

G.Patton

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Čestitamo. Ali ste ga objavili tukaj, da bi promovirali svojo osebno svetovalno službo, ali pa želite deliti svoje misli?
 

w2x3f5

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Hidroliza je bila izvedena pod mojim vodstvom in po moji metodi Heisenblack. Mislim, da bo metodologijo objavil pozneje, po povečanju obsega
 

w2x3f5

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pred objavo je treba preveriti ponovljivost
 

Heisenblack

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Da, metodologijo bom objavil po izvedbi 50gr serije, 12ml p2p iz 20 gr natrijevega glicidata je bilo suhih
 

G.Patton

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Lepo je to prebrati =) Hvala.
 

G.Patton

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Pravzaprav nimam pojma, kaj je to. Nikoli še nisem poskusil metode s fosforno kislino z refluksom.
 

w2x3f5

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pregrevanje je zelo verjetno, keton zlahka oksidira, možne so dodatne stranske reakcije
 

blackburn

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Da, to je 5449-12-7 @G.Patton

@w2x3f5 okey dobro moram poskusiti moj način ...

Hvala obema
 

w2x3f5

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pišite mi v zasebna sporočila, lahko samostojno preverite metodo, preverite rezultat. nenadoma se bodo pojavile pasti
 

Re186

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Približno čez teden dni bom poskusil sintezo na skali od benzaldehida do BMK do P2P, nameravam refluksirati žveplovo kislino, ki jo je v članku navedel @G.Patton, takrat bom delil svoje mnenje in objavil izvirne eksperimentalne podatke
 

metux

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Ali lahko uporabim olje rjavo rdeče barve, za redukcijo?
 

Heisenblack

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Rjavo rdeče obarvano olje je nereagirana glikidna kislina, najbolje bi bilo, da keton destilirate s paro in ga nato uporabite v naslednjem koraku
 

Megido

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Mislim, potem imate olje, vendar to olje 6 mesecev staro in postane rdeče barve,. Ali moram v naslednjem koraku ponovno destilirati?
 
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