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I will share the table with you.
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I will share the table with you.
View attachment 7998
Keep it below 180, better below 175°C and calibrate the Infrared thermometer to the flask/setting you use or you will never exactly know how hot it is.
Good luck
↑View previous replies…
OrgUnikumWait a second.. @OrgUnikum does that mean that after drying the methylene chloride you can potentially just start adding D-(-)-Tartaric acid (cas 147-71-7) and participating d-meth salt??
If so is there anymore literature on microwave irradiation? You guys are worth your weight in gold thank you.
Throw-offPlenty literature but be aware that the trick is less the Microwaves but that this is a pressure vessel in a micro and the pressure makes it happen. I realized this myself only lately: The key to a successful Leuckart reaction for Amphetamine is to use a pressure vessel for reaction and hydrolysis. Methamphetamine can be made by the Leuckart without pressure vessel, yields are not stellar though, Al/Hg or NaBH4 is far better for this.
And separation of the Stereoisomeres, of d- meth and l-meth is not as easy as adding D-(-)-Tartaric acid, sorry. But there is no need for the rare and expensive D-(-)-Tartaric acid, the normal tartaric acid, the natural derived one, can be used. The process involves the natural tartaric acid 1/4 mol, HCl 1/2 mol, d/l-meth 1 mol and involves salt formation and partial dissolution/reformation of the salt (ripening) until virtually complete separation is achieved. Not trivial. Very temperature and setup dependent AFAIK.
OrgUnikumWhen you say yields are not stellar what type of percentage are we talking? Is it not similar too the study above with the Methly derivative of formamide?
The reason for the use of D-(-)-Tartaric instead of the natural derived one is because I have it readily available and free. The solid mass is the D isomer and the solution is the L isomer correct?
Throw-offNever mind about the Tartaric question, I worked it out today. Thanks friend.
OrgUnikumWith Hydrolysis of the formyl amide in these measurements.
NMF - 130ml
P2P - 100ml
Formic - 84ml
How much naoh solution do you need and how much HCI? Is 35% lab grade sufficient?
I attach the article and you can look for yourself. I saw a post elsewhere where somebody claims good yields like 80% in a modified household microwave(hole for condenser) with temperatures not over 175°C to avoid Formamide decomposition. No further details were given on this.
If so is there anymore literature on microwave irradiation? You guys are worth your weight in gold thank you.
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Wait a second.. @OrgUnikum does that mean that after drying the methylene chloride you can potentially just start adding D-(-)-Tartaric acid (cas 147-71-7) and participating d-meth salt??
If so is there anymore literature on microwave irradiation? You guys are worth your weight in gold thank you.
And separation of the Stereoisomeres, of d- meth and l-meth is not as easy as adding D-(-)-Tartaric acid, sorry. But there is no need for the rare and expensive D-(-)-Tartaric acid, the normal tartaric acid, the natural derived one, can be used. The process involves the natural tartaric acid 1/4 mol, HCl 1/2 mol, d/l-meth 1 mol and involves salt formation and partial dissolution/reformation of the salt (ripening) until virtually complete separation is achieved. Not trivial. Very temperature and setup dependent AFAIK.
Plenty literature but be aware that the trick is less the Microwaves but that this is a pressure vessel in a micro and the pressure makes it happen. I realized this myself only lately: The key to a successful Leuckart reaction for Amphetamine is to use a pressure vessel for reaction and hydrolysis. Methamphetamine can be made by the Leuckart without pressure vessel, yields are not stellar though, Al/Hg or NaBH4 is far better for this.
And separation of the Stereoisomeres, of d- meth and l-meth is not as easy as adding D-(-)-Tartaric acid, sorry. But there is no need for the rare and expensive D-(-)-Tartaric acid, the normal tartaric acid, the natural derived one, can be used. The process involves the natural tartaric acid 1/4 mol, HCl 1/2 mol, d/l-meth 1 mol and involves salt formation and partial dissolution/reformation of the salt (ripening) until virtually complete separation is achieved. Not trivial. Very temperature and setup dependent AFAIK.
The reason for the use of D-(-)-Tartaric instead of the natural derived one is because I have it readily available and free. The solid mass is the D isomer and the solution is the L isomer correct?
When you say yields are not stellar what type of percentage are we talking? Is it not similar too the study above with the Methly derivative of formamide?
The reason for the use of D-(-)-Tartaric instead of the natural derived one is because I have it readily available and free. The solid mass is the D isomer and the solution is the L isomer correct?
Maybe it is just fair to add that temperatures over 180 °C like the named 200 and 210 °C for sure completely destroy P2P and even the Formamide, the resulting vapors and gases are highly toxic. Vent everything coming from top of the condenser outsides! Seriously!
Keep it below 180, better below 175°C and calibrate the Infrared thermometer to the flask/setting you use or you will never exactly know how hot it is.
Good luck
NMF - 130ml
P2P - 100ml
Formic - 84ml
How much naoh solution do you need and how much HCI? Is 35% lab grade sufficient?
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I will share the table with you.
View attachment 7998
Formamide 50 ml 1,5 mol
formic acid 56 ml 1,5 mol
P2P 66 ml 0,5 mol
↑View previous replies…
OrgUnikumWhen using N-Methylformamide is 89.5ml 1.5 mol in your ratio @OrgUnikum
Throw-offYou look up the molekular weight of N-Methylformamide - mol/g - on Wikipedia and multiply by 1,5 as seen in the post of mine you refer to. I am not going to do this for you.
And as a free service from yours truly, the ratios for P2P:
Formamide 50 ml 1,5 mol
formic acid 56 ml 1,5 mol
P2P 66 ml 0,5 mol
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When using N-Methylformamide is 89.5ml 1.5 mol in your ratio @OrgUnikum