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Hive BB  Chemistry
Discourse  Sassafras
into Isosafrole
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| Author | Topic: Sassafras into Isosafrole |
| HELTERSKELTER unregistered |
 posted 09-02-98 04:18 PM
I was wondering if someone could post an easy method on changing Sassafras oil into Isosafrole. All the help would be appreciated! |
| ketone Member |
posted 09-02-98 05:13 PM 
Distill the oil and save the safrole fraction. Take this, some anhyr. EtOH and some KOH and reflux. Extract with a suitable organic solvent. Distill off solvent. Bingo, you have isosafrole. Easy enough? -ketone |
| HELTERSKELTER unregistered |
posted 09-02-98 06:49 PM
O.k. now,how much of each? Material wise. Thanx! |
| ketone Member |
posted 09-02-98 07:20 PM
I don't want to appear rude, but I really think you should invest in a copy of TS II...if you need to know the quantities you've probably got a multitude of other questions and probably need more details on these procedures. It's be $35 well spent, trust me. Anyway (stright from TS I), reflux 100g safrole, 100mL anhydr. EtOH and 200g KOH for 12-24hrs. Distill off EtOH, add 500mL dH2O, extract with DCM. Remove DCM by distillation. Add parsley for decoration. Serves 4. -ketone |
| sparks Member |
posted 09-03-98 02:24 AM
About this izomerisation..... Is anhydr. meOH as useful as anhydr. etOH ? The bp. is a bit lower...but does it really matter ? And one last thing: will fresh oregano do instead of parsley....maybe even some chocolate chips would be better.... |
| Arthur
Bach Member |
posted 09-03-98 05:29 AM
You might want to check out Rhodium's site, look for " Eleusis safrole isomerization 1.5 " That way seems a little easier . Peace..AB |
| jamex Junior Member |
posted 09-03-98 08:58 AM
will denatured EtOH with methanol in it fuck it up? jamex |
| quirks Member |
posted 09-03-98 10:00 AM
10g CaOH, ~1g NaOH/KOH, CaOH, NaOH from the hardware store. |
| jamex Junior Member |
posted 09-03-98 11:56 AM
quirks: I am familiar with the different routes, but still would like to know if there has been success/failure with EtOH with methanol in it. Caked on tar is hard to remove from glassware. still haven't gotten that mail from you. did you recieve anything from me? jamex |
| r2d3 Member |
posted 09-04-98 01:23 PM
A foaf put 7g of KOH into 400g of warm safrole and reluxed under aspirator at 122-135C for 4hr. The reflux set-up was swapped for distillation and 364g of iso was collected with NO forerun. About 50ml of 25% NaOH was put into the flask and gently heated for 5min. Clean as a whistle.The foaf wants to send a big thanks to OS. |
| The
Alchemist Member |
posted 09-06-98 02:38 PM
quirks, I thought it was CaO/KOH that was used in the isomerization? |
| Rhodium Administrator |
posted 09-06-98 07:03 PM
Correct, it is CaO/KOH. The CaO reacts with the 15% water in the KOH forming Ca(OH)2, making the reaction anhydrous. |
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