Hi, guys!
Just in case anyone is still interested in making EtNO2 or MeNO2 some easy OTC way :) ...
I found a patent (2,105,581) on uspto.gov that describes preparation of nitromethane from CH3Cl and aq. NaNO2. Methyl chloride is bubbled into vigorously boiling sat. NaNO2 soln. at pH 6-10 (CaCO3 used as buffer) with stirring (it says "suitable means of securing intimate contact between gas and the soln.") and preferrably a foaming agent (any form of soap) to increase the rxn surface. Nitromethane is continuously fractionally distilled from the rxn as its azeotrope w/water (bp 82 C) - it slows down the rxn if it's not. Additional water and NaNO2 should be periodically added to the rxn mixtr.
The patent says the invention may be applied for production of any other alkylnitrate as well. It doesn't state the yield specifically, but it's been my impression that it's high since a) the proc. was developed as an industrial process of MeNO2 manufctring b) only 10% of methyl nitrite is formed. So... Here you go, my beloved fellow bees. As easy as it gets. That is, if it works - i tend to cross my fingers lately when i say smth like this :)
SWIM won't be around for 2 or maybe three weeks so he can't check it right now. Maybe some people you met (esp. the ones possessing stirrer hotplates ;) ) can do a trial run or two of this inexpensive and promising procedure?
Here's the link to the full patent image (AlternaTiff plug-in required): http://patimg2.uspto.gov/.piw?Docid=02105581&homeurl=http%3A//164.195.100.11/netacgi/nph-Parser?Sect1=PTO1&Sect2=HITOFF&d=PALL&p=1&u=/netahtml/srchnum.htm&r=1&f=G&l=50&s1=%272%2C105%2C581%27.WKU.&OS=PN/2%2C105%2C581&RS=PN/2%2C105%2C581&PageNum=&Rtype=&SectionNum=&idkey=1B10F8A8CC23 (http://patimg2.uspto.gov/.piw?Docid=02105581&homeurl=http%3A//164.195.100.11/netacgi/nph-Parser?Sect1=PTO1&Sect2=HITOFF&d=PALL&p=1&u=/netahtml/srchnum.htm&r=1&f=G&l=50&s1=%272%2C105%2C581%27.WKU.&OS=PN/2%2C105%2C581&RS=PN/2%2C105%2C581&PageNum=&Rtype=&SectionNum=&idkey=1B10F8A8CC23)
(jesus is it supposed to be that long???)
and the .tiff plug-in (190 Kb):
http://www.mieweb.com/alternatiff/distribution/alternatiff-1_3_7.exe (http://www.mieweb.com/alternatiff/distribution/alternatiff-1_3_7.exe)
Thank you all in advance,
Antoncho
between making an alkyl nitrite and an alkyl nitrate
Don't you mean nitroalkane (RNO2) rather than alkyl nitrate (RNO3)?