Author Topic: A few Q's b4 wacker...  (Read 3688 times)

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VinnyC

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A few Q's b4 wacker...
« on: May 30, 2001, 02:15:00 PM »
Ok, SWIM (if not too tired 2nite) will be dreaming of step 3 of Bright Star and would like to know a couple things.
1) Although he has seen it mentioned in various places he just wants to double check to be sure... He can substitue MeOH for DMF throughout this step (but use same amounts i.e. 300ml and then 50ml MeOH) correct?
2) If MeOH is fine to use, SWIM has a "heet" substitue that has a flourescent green hue to it. SWIM thinks it may be just a dye. Would this cause a problem to use?
3) The dripping of the safrole/MeOH mix should be done over 30 min. SWIM figures he can use his sep funnel opened just a bit to get the dripping, but wonders how many drops/sec he should shoot for. Or is there some other guideline he should follow?

Thanks!


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spric

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Re: A few Q's b4 wacker...
« Reply #1 on: June 04, 2001, 05:50:00 PM »
350-400ml MeOH/ 2g pdcl2.  dmf is bad, sucka.  If you went this far, why don't you spend an hour distilling your heet?  And if you can get DMF, how bout methanol?  I can find the ref and don't know if it matters, but it is bad to slop all the safrole in at once, unless it is added and water is dripped in over a few hours(variation no one cares about).  Either way it will work, just drip it over 30-45 min while your plate reaches the desired temp.  and no synthesis is complete without newcastle in your ice bath and green in your bong.


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