Can someone please confirm this route for isolating safrole from sassafras oil.
1) Treatment with 5% NaOH
Treate sassafras oil with an equal amount of 5% NaOH solution (I'm assuming this solution is calculated by weight, for example 25g NaOH + 475g dH2O). This will create eugenol anion crystals in the water layer, which is decanted from the oil. Wash the remaining oil with 3X dH2O and decant the water layers from each washing.
Transfer oil to a cooking pot and raise temp. to 100C to remove excess water.
2) Distillation of safrole
Set up for simple vacuum distillation. If the vacuum pulls 20mm, then the following should occur under slow and controlled heating conditions...
at ~55C, pinene distills over
at ~70C, phellandrene distills over
at ~100C, d-camphor distills over
Once the remaining d-camphor distills over, the tempurature of the distilling flask will begin to rise to the bp of safrole under vacuum at 20mm, namely, 125C. At this point, the contents of the distilling flask can be considered relatively pure safrole.
Look ok?