Author Topic: ccl3 ok in performic?  (Read 1334 times)

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abc123

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ccl3 ok in performic?
« on: November 04, 2001, 11:12:00 PM »
i see no problems in using ccl3 rather than dcm in a buffered performic as long as the temp stays about 40c correct?

abc123

sunlight

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Re: ccl3 ok in performic?
« Reply #1 on: November 05, 2001, 05:02:00 AM »
Probably it won't affect too much. Try it and tell us.

abc123

  • Guest
Re: ccl3 ok in performic?
« Reply #2 on: November 05, 2001, 01:40:00 PM »
it seems to be fine but it kinda sucks because DCM boils about 40c and boiling is a cooling process so the damn chloroform is taking forever to add. even if it sits for an hour without any adding performic, the temp barely drops

beside that i think it will work fine...will post later

abc123

Chromic

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Re: ccl3 ok in performic?
« Reply #3 on: November 05, 2001, 03:13:00 PM »
Cooling bath??

abc123

  • Guest
Re: ccl3 ok in performic?
« Reply #4 on: November 06, 2001, 11:07:00 AM »
swim thought that too and had bad results a while back (with DCM so it could be added faster)...swim posted that same question on rhodiums peracid review post and zooligan said no (about DCM not ccl3).

  an icebath may work here because the heat loss to the ice could possibly be somewhat equivelent to the heat loss from boiling ...if an ice  bath is used sparingly....would have tried it but it was stuck in swim's head that ice baths are bad...wish he did try because that dripping took forever and several times the temp went up above 40

ice baths are bad with DCM but maybe not here?

thanks

and big bottles of DCM suck because so much is lost just due to opening the bottle...next time swim will divide DCM into a bunch of smaller botlles or keep the damn thing cold

abc123

LaBTop

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Re: ccl3 ok in performic?
« Reply #5 on: November 07, 2001, 06:39:00 AM »
Read the last NEW performic post in my sticky thread (It's DONE) and you will see that DCM is the best to use because it boils at 40 C.
Patience during dripping is the way to go. LT/

WISDOMwillWIN

abc123

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Post deleted by Rhodium
« Reply #6 on: November 07, 2001, 10:37:00 AM »

baalchemist

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Re: ccl3 ok in performic?
« Reply #7 on: November 07, 2001, 10:15:00 PM »
If one has all the correct chems to begin with to run a particular reaction, why in the hell would you want to
try substituting a crucial ingredient with something else?
To speed up the addition process? or trying to re-invent the wheel. Ever hear of an addition funnel? Baal sets his to 1-2 drips per second and moves on to better things for 24hrs.

If your DCM is evap'ing that quickly, you must live in a desert or something.  

GODISNOWHERE

Antibody2

  • Guest
Re: ccl3 ok in performic?
« Reply #8 on: November 07, 2001, 11:09:00 PM »
you getting mellow baal?

"All those memories lost like rain..."

abc123

  • Guest
Re: ccl3 ok in performic?
« Reply #9 on: November 08, 2001, 12:35:00 AM »
1. DCM wasnt available at that time and swim saw no reason not to use chloroform ..swim did NOT want to use ccl3....so the original question was asked==> did anyone see any problems using ccl3. if dcm was present it WOULD have been used. swim did not want to use ccl3 just to see how it would act in a performic or to try to change how the performic is done

2. nothing was trying to be invented...durring a period without DCM, swim saw no reason to not experiment with other possible options and didnt want to play with jellied DCM that gives DCM + azeotropes......==>whats better no rxn for the few days without DCM? or is it beter to run a rxn that involves a longer dripping time, for the few days without DCM?

3. an addition funnel when using DCM works perfectly as you stated but without the cooling caused by the boiling of DCM the addition of the performic takes much longer...it also  took 24 hours with ccl3 but swim would guess his rxn was much smaller (140g iso)...swim has heard of an addition funnel by the way...(actually swim hooked 2 addition funnels up so when swim's nobody went to work, that nobody could resume the dripping by turning the second one on, so swims lazy ass could sleep without having to get up and fill the funnel again...the second funnel was covered with foil to reduce light absorption

4. desert?...swim said that lots is lost due to opening it (swim wasnt very clear)...a gallon of DCM at room temp (70F)when opened releases pressure..thats DCM escaping...i guess the word "lots" is relative because if the gallon was divided into smaller containers some would be saved (OK your right, a large percentage isnt lost)...swim would guess at least 5% (maybe more )is lost by the time the bottle is empty...lots meaning===>the DCM lost due to evap from opening bottle is allot more than say the amount of solvent lost when opening most other solvents.

baalchemist: swim wasnt or isnt trying to piss you off...he was only asking others for their opinion on a temporary problem....

[it may not be all bad either, perhaps a better yeild could be obtained because much of the heat lossed per unit time in the rxn when using DCM is caused by boiling but the heat lost per unit time in the ccl3 rxn is mainly caused by the rxn's thermal contact with its surronding...so if both types (DCM and CCl3) are held at 40c, the chloroform one would have an internal energy that is equal but would have this energy for a longer period..maybe it is good/maybe-not..the same thing would happen with DCM if the temp wasnt allowed to reach reflux.......swim has no idea if this would be better, worse, or make no difference at all]??????

 this ^ was by no means his purpose for using chloroform actually swim didnt want to use it but the benfits outweighed the consequences which was about 10 hours extra dripping

like swim said, he was only asking for opinions..he wasnt trying to invent any wheel..sorry if swim offended you baalchemsit...it wasnt his objective

abc123