02-14-03 11:04
No 407830
I've been very interested in using Grignard reagents for some of the synthesis posted on the hive but I've found it a problem getting Magnesium.
The only place that looks promising in the UK and doesn’t just sell ribbon has minimum order of 57 kilo of (150 to 200 mesh) powder.
I've been thinking of the reduction of magnesium sulphate with sodium made by electrolysis.
I've thought of mixing the two then under an argon atmosphere at about 100c going as far up as 650c or 700c to allow the Mg to sink to the bottom of a stainless steel pot or cylinder. Or would it????
If it were possible to do it that way would the NaSO4 be a problem when added along with Mg in a Grignard reagent????
Another question to any one that might have an answer, if you need to make carbonyl chloride but don’t have thionyl chloride can you use phosgene gas I’m wondering because the easy with which it can be made and the similarity between phosgene and thionyl chloride.
I know that it is a very dangerous gas (was used in one of the world wars) so no one would advise the use of it but if Phosgene could be used and the Magnesium can be reduced then I see there being no need to ever contact a chemical supply store again.
(Hive Addict)
02-15-03 03:29
No 408104
I don´t know if Na and MgSO4 would react but those conditions are nasty. That has to answered by another bee. Thionyl chloride could be substituted with phosgene, but also with oxalyl chloride. You do not want to mess with phosgene. You will most likely end up killing yourself, or worse, someone else. Get thionyl chloride or oxalyl chloride, or make them yourself.
Freaky
(Stranger)
02-15-03 13:23
No 408244
I've just searched the "Fucking search engine" and found reference to phosgene and the production of thionyl chloride.
Nice one
. Thank you.(Hive Bee)
02-17-03 07:27
No 408983
You live in the UK and can get hold of phosgene, sodium, argon, anhydrous ether and everything required for your Grignard reaction apart from magnesium? Grignard reagents are difficult to work with as it is, and home-made magnesium won't help matters at all. I suggest you steer well away from your current plan and look for another source of magnesium. If you can't find one you'll have plenty of problems with aquisition of more suspicious items later.
I can't imagine even enquiring about phosgene, and making your own would be suicide (literally!). If you can get sodium by electrolysis, couldn't you just as easily get lithium from a lithium salt? This could then be used as is to replace your Grignard with an organolithium reagent and do away with magnesium altogether; these reagents can often be interchanged, depending on which synthesis you are planning.
Still, I seriously suggest finding a commercial source for Mg turnings, which is far less suspicious than many others items you'll need for a Grignard reaction. Good luck
(Distinctive Doe)
02-17-03 22:35
No 409243
Has anyone successfully used the magnesium from a magnesium firestarter for a Grignard?
(Hive Bee)
02-18-03 08:49
No 409419
The same can be asked of filings drilled from a hard drive chassis or an old VW gearbox.
But seriously, old computer hardware can be had easily. Post 108478 (dormouse: "Oxime->amine with Zn-Ni couple. (Page 1) -Labrat", Novel Discourse):
BTW to obtain reasonably pure magnesium, look no farther than your automotive boneyard.
Yep! Old VW tranny boxes are magesium. (personal experience). An electric drill will yeild all the Mg turning you require.