swim's first oximation dream ended up with a green jellyfish blob that he couldn't do anything with.
swim changed some parameters and then he got an aldoxime that was white (with a hint of yellow) and very sticky/tacky. need it to solidify to the point where its no longer sticky because of all the mechanical losses of it sticking to everything. washed it several times with water but it refused to solidify (it's insoluble in water). it would become immobilized/solidify in the freezer but upon thawing out would return to the same consistency as before. swim saw that covering it in 70% IPA (it is insoluble in water but slightly soluble in IPA) allowed it to solidify to something that looked like cottage cheese except perhaps a little more stringy looking, not crystalline but definitely a solid and no longer sticky, it was clumpy as in it clumped to itself like cottage cheese in appearance but it wasn't sticky so no mechanical losses to the surface of things it touches. a little more H2O was added to the IPA to dilute it more and decrease solubility of the aldoxime in the IPA. the IPA was then removed whatever impurity was keeping the oxime sticky. the IPA was pipetted off and kept in a separate beaker, then the oxime was put under a fan to dry out. the IPA in the beaker was yellowish orangeish and the oxime was off-white.
as the oxime dried under the fan it began to turn dark, a dark green in fact.... weird. the IPA, over the course of a day, began to clear up to a light milky white/yellow color and on the bottom of the beaker was a nasty dark orange viscus oil. why an off-white cottage-cheese-solid aldoxime turned dark green when being dried over a fan swim has no idea
swim wasn't sure just how much oxime was lost (dissolved) in the IPA so he poured the beaker with the IPA and viscus oil back onto the oxime to start from scratch again. would a method like recrystallization help purify this oxime? the oxime is fairly soluble to warm MeOH and a little less soluble in IPA he thinks (he assumes this from some very crude, quick tests the other day), adding water helps push the oxime out however it seems to be easier to precipitate the oxime out of IPA than MeOH, he may be wrong as that is what he's assuming from a quick test.
he's thinking of trying crystallization using hot alcohol (IPA or MeOH) but read of a different oxime being recrystallized from hexane. swim doesn't have hexane but he has heptane he can try (h**p://www.erowid.org/archive/rhodium/chemistry/alpha-deuterio.amphetamine.html)
swim has been trying to get it to solidify as a white solid (is it crystalline in its purest form?) at room temp without much success
swim changed some parameters and then he got an aldoxime that was white (with a hint of yellow) and very sticky/tacky. need it to solidify to the point where its no longer sticky because of all the mechanical losses of it sticking to everything. washed it several times with water but it refused to solidify (it's insoluble in water). it would become immobilized/solidify in the freezer but upon thawing out would return to the same consistency as before. swim saw that covering it in 70% IPA (it is insoluble in water but slightly soluble in IPA) allowed it to solidify to something that looked like cottage cheese except perhaps a little more stringy looking, not crystalline but definitely a solid and no longer sticky, it was clumpy as in it clumped to itself like cottage cheese in appearance but it wasn't sticky so no mechanical losses to the surface of things it touches. a little more H2O was added to the IPA to dilute it more and decrease solubility of the aldoxime in the IPA. the IPA was then removed whatever impurity was keeping the oxime sticky. the IPA was pipetted off and kept in a separate beaker, then the oxime was put under a fan to dry out. the IPA in the beaker was yellowish orangeish and the oxime was off-white.
as the oxime dried under the fan it began to turn dark, a dark green in fact.... weird. the IPA, over the course of a day, began to clear up to a light milky white/yellow color and on the bottom of the beaker was a nasty dark orange viscus oil. why an off-white cottage-cheese-solid aldoxime turned dark green when being dried over a fan swim has no idea
swim wasn't sure just how much oxime was lost (dissolved) in the IPA so he poured the beaker with the IPA and viscus oil back onto the oxime to start from scratch again. would a method like recrystallization help purify this oxime? the oxime is fairly soluble to warm MeOH and a little less soluble in IPA he thinks (he assumes this from some very crude, quick tests the other day), adding water helps push the oxime out however it seems to be easier to precipitate the oxime out of IPA than MeOH, he may be wrong as that is what he's assuming from a quick test.
he's thinking of trying crystallization using hot alcohol (IPA or MeOH) but read of a different oxime being recrystallized from hexane. swim doesn't have hexane but he has heptane he can try (h**p://www.erowid.org/archive/rhodium/chemistry/alpha-deuterio.amphetamine.html)
swim has been trying to get it to solidify as a white solid (is it crystalline in its purest form?) at room temp without much success