Post 511869 (https://www.thevespiary.org/talk/index.php?topic=10688.msg51186900#msg51186900)
(Barium: "You can make the alkoxides by dissolving e.g.", Newbee Forum)Post 511982 (https://www.thevespiary.org/talk/index.php?topic=10688.msg51198200#msg51198200)
(Organikum: "Process without distillation", Newbee Forum)Post 512000 (https://www.thevespiary.org/talk/index.php?topic=10688.msg51200000#msg51200000)
(gsus: "precipitation with acetone, alleged", Newbee Forum)Post 512006 (https://www.thevespiary.org/talk/index.php?topic=10688.msg51200600#msg51200600)
(Nicodem: "The patents work", Newbee Forum)Post 511960 (https://www.thevespiary.org/talk/index.php?topic=10688.msg51196000#msg51196000)
(Organikum: "Barium, do you know the composition and bp of...", Newbee Forum)Post 466982 (missing)
(psyloxy: "practical alkyl tosylate synth - new approaches", Novel Discourse)Patent US2451945 (http://l2.espacenet.com/dips/viewer?PN=US2451945&CY=gb&LG=en&DB=EPD)
, only regenerate-able mol sieves are substituted for acetylene producing calcium carbide.Patent DE628023 (http://l2.espacenet.com/dips/viewer?PN=DE628023&CY=gb&LG=en&DB=EPD)
I think it can be taken for granted that the percentage of water in the vapor-phase is low because the equilibrium lies heavily on the left (little water is generated by NaOH + MeOH __> NaOMe + H2O) thus the difference in boiling points of MeOH and MeOH/H2O is small, a few °C if you're lucky. What big ass fractionation column did those crazy Germans think of ?Dynamic drying: solvent is filtered thru a chromatography column. 250g mol sieves are sufficient to dry 10L of solvent to a water content of 0.002% (20ppm). Column: 2.5 x 60cm (~1"x23"). Throughput: 3L/h. (transl from : www-oc.chemie.uni-regensburg.de/OCP/methoden/kap9.PDF )
Mol sieves have a capacity of ~20% their own weight, so you would need ~ 100g mol sieves for every 54g NaOMe.
Any objections ?
--psyloxy--
it should have the consistency of wet concrete.
Because of the mol sieves or the NaOMe ? After all 30% NaOMe/MeOH is commonly referred to as 'solution' - that's what I took it for being.
However, using a Soxhlet, or more MeOH for that matter, should solve that problem. ;)
--psyloxy--
Patent DE1043309 (http://l2.espacenet.com/dips/viewer?PN=DE1043309&CY=gb&LG=en&DB=EPD)