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All 5 posts Subject: MD-P2P formic acid method Please login to post Down

saffrole
(Stranger)
02-03-04 07:44
No 486148
      MD-P2P formic acid method

I have a quick question on the safrole-MD-P2P method using formic acid and H2SO4 (I beleive method 1 in Strike's book- the one listed as "Strike's favorite") In the illustration, it shows safrole to MD-P2P, but the text lists iso-safrole as the starting material. Does this mean that either will work? Or does one work better than the other or one not at all. Anyone with experience in this (indirect, of course)- your help will be greatly appreciated, as I'm about to dream about this one soon (and this dream consists of, not surprisingly, very limited safrole)
In case anyone reads this, I am deranged and dont know what I'm talking about.

Bandil
(The Archetypical "Good Guy")
02-03-04 08:41
No 486154
      Safrole is the starting material.

Safrole is the starting material. This is isomerized to isosafrole which can be used in the performic acid ketone synthesis. Using safrole directly will result in zero to slim yields (so no, safrole can not be used directly in this synthesis).

The isomerization process is really easy. Simply reflux safrole with 1-2% KOH or NaOH present at atmospheric pressure for 12 hrs and you will have 90%+ isosafrole (you obvisously need to distill after the isomerization process).

Regards
Bandil

Drugs = Fun; Drugs <> Money

saffrole
(Stranger)
02-03-04 11:42
No 486176
      thanks

I figured that out later in the night- (I rearranged the words I was putting into TFSSE)Seems simple enough. I am just glad that no one yelled at stupid-ass me about that FSE!

sassypants
(Newbee)
03-24-04 07:31
No 497003
User Picture       Trying to isomerize

SWIM has been trying to isomerize for about the last 3 weeks... was trying Bandil's method stated above. made sure to let the water all boil out before slapping on the condenser, then tried refluxing at atm pressure for ~10hrs. Well, the other day, SWIM's high-quality proper lab thermometer with range up to ~300 finally shows up. Apparantly, the whole set-up has probably never gotten hot enough in all the isomerization attempts. So today SWIM tried a new isomerization, same set up as before, except covered the oil bath and flask and base of the condenser with foil, then left for about 7 hours, since it apparantly takes a good couple hours for the oil bath to get to a near acceptable temp. SWIM came back and turned the heat off, after determining the temp was now over 250 C. Then had to leave again. Will have to deal with the gooey mess tomarrow. Is it normal to have gloppy looking end product? (almost like saponification product)
Also, is it possible that SWIM's small laboratory stirrer/hotplate is just not powerful enough? Last question: SWIM heard that running cool (not cold)water through the condenser is not a wise choice here, due to breakage risk. Is this really true? Thought that lab glass was made to handle this kind of stuff.

Distill. Isomerize. Distill. Oxidize. Distill. Reduce. Crystalize. Repeat.

Rhodium
(Chief Bee)
03-24-04 16:39
No 497056
User Picture       inadequate lab gear

Also, is it possible that SWIM's small laboratory stirrer/hotplate is just not powerful enough?

That is very likely.

^{The Hive - Clandestine Chemists Without Borders}

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	All 5 posts		Subject: MD-P2P formic acid method		Please login to post		Down


		saffrole (Stranger) 02-03-04 07:44 No 486148				MD-P2P formic acid method
						I have a quick question on the safrole-MD-P2P method using formic acid and H2SO4 (I beleive method 1 in Strike's book- the one listed as "Strike's favorite") In the illustration, it shows safrole to MD-P2P, but the text lists iso-safrole as the starting material. Does this mean that either will work? Or does one work better than the other or one not at all. Anyone with experience in this (indirect, of course)- your help will be greatly appreciated, as I'm about to dream about this one soon (and this dream consists of, not surprisingly, very limited safrole) In case anyone reads this, I am deranged and dont know what I'm talking about.



		Bandil (The Archetypical "Good Guy") 02-03-04 08:41 No 486154				Safrole is the starting material.
						Safrole is the starting material. This is isomerized to isosafrole which can be used in the performic acid ketone synthesis. Using safrole directly will result in zero to slim yields (so no, safrole can not be used directly in this synthesis). The isomerization process is really easy. Simply reflux safrole with 1-2% KOH or NaOH present at atmospheric pressure for 12 hrs and you will have 90%+ isosafrole (you obvisously need to distill after the isomerization process). Regards Bandil Drugs = Fun; Drugs <> Money



		saffrole (Stranger) 02-03-04 11:42 No 486176				thanks
						I figured that out later in the night- (I rearranged the words I was putting into TFSSE)Seems simple enough. I am just glad that no one yelled at stupid-ass me about that FSE!



		sassypants (Newbee) 03-24-04 07:31 No 497003				Trying to isomerize
						SWIM has been trying to isomerize for about the last 3 weeks... was trying Bandil's method stated above. made sure to let the water all boil out before slapping on the condenser, then tried refluxing at atm pressure for ~10hrs. Well, the other day, SWIM's high-quality proper lab thermometer with range up to ~300 finally shows up. Apparantly, the whole set-up has probably never gotten hot enough in all the isomerization attempts. So today SWIM tried a new isomerization, same set up as before, except covered the oil bath and flask and base of the condenser with foil, then left for about 7 hours, since it apparantly takes a good couple hours for the oil bath to get to a near acceptable temp. SWIM came back and turned the heat off, after determining the temp was now over 250 C. Then had to leave again. Will have to deal with the gooey mess tomarrow. Is it normal to have gloppy looking end product? (almost like saponification product) Also, is it possible that SWIM's small laboratory stirrer/hotplate is just not powerful enough? Last question: SWIM heard that running cool (not cold)water through the condenser is not a wise choice here, due to breakage risk. Is this really true? Thought that lab glass was made to handle this kind of stuff. Distill. Isomerize. Distill. Oxidize. Distill. Reduce. Crystalize. Repeat.



		Rhodium (Chief Bee) 03-24-04 16:39 No 497056				inadequate lab gear
						Also, is it possible that SWIM's small laboratory stirrer/hotplate is just not powerful enough? That is very likely. ^{The Hive - Clandestine Chemists Without Borders}

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