All the experimental procedures I have seen for the production of 1-(2,5-dimethoxyphenyl)-2-nitroethane describe the product as a yellow oil.
Is it possible to crystallize this oil from absolute ethanol?
Two samples of this compound that were produced according to Barium's EtOAc/ethanol method to be found at:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/nitrostyrene.nabh4.reduction.html
One of these samples smelt somewhat of acetic acid at the end of the procedure, and was therefore washed with dH2O (the oil was washed directly with dH2O and was not then extracted with organic solvent, dried and evaporated). It can be assumed that this sample therefore contained some water.
This sample, and another, were both dissolved in separate portions of boiling absolute ethanol.
On cooling, the wet sample has formed some white crystals and the remaining mother liquor is bright yellow. Further cooling of this solution causes a yellow goo to fall out of solution around the white crystals.
The other sample (the dry one) fails to form crystals on cooling even when seeded with one of the white crystals from the wet sample recrystallization.
Can anyone enlighten me as to the mp. of 1-(2,5-dimethoxyphenyl)-2-nitroethane please?
Are the white crystals that have fallen out of the first sample likely to be 1-(2,5-dimethoxyphenyl)-2-nitroethane or something else (e.g. ketone from an undesired nef reaction)?
Has anyone here ever recrystallized 1-(2,5-dimethoxyphenyl)-2-nitroethane and if so, from what solvents/ratios?
Many thanks for your help.