synthesis by raffike from the vespiary :3
pls note that Fe(CO)5 is super toxic and "it's recommended to do the reaction under a fume hood or with good ventilation"
Reagents:
ᗢ 500 grams of safrole distilled from Ocotea Cymbarum
ᗢ 3 grams of technical +98,5%NaOH
ᗢ 3 grams of lab grade Fe(CO)5 from Fluka
Procedure:
500 grams of safrole was put in a 2 liter round bottom flask that was sitting on a heating mantle. Overhead stirring was applied and 3 grams of NaOH and 3 grams of Fe(CO)5 were added. Started heating. Somewhere at 110 degrees C, obvious exothermic reaction kicked in, just like described in Rhodium's isomerization review, and heating was turned off. 15 minutes passed and stirring was turned off and flask was allowed to cool down. When flask was cooled, dark organic mixture was washed with 200 mls 20% acetic acid and then with 200 mls water. Some emulsion formed but that cleared up in about and hour and then organic layer was sepped off with 1 liter separatory funnel. Organic mixture was poured to 2 liter flask, attached claisen still head and liebig condenser with vacuum adapter. Receiving flask was 1 liter round bottom. Vacuum applied and started heating. From 114 C to 118 C at 10 mm vacuum only fraction came over which was almost colourless.
Final yield: 456 grams which means +90% yield. There were some losses during the washes that will be avoided next time and I think +95% yield isn't hard to obtain.
pls note that Fe(CO)5 is super toxic and "it's recommended to do the reaction under a fume hood or with good ventilation"
Reagents:
ᗢ 500 grams of safrole distilled from Ocotea Cymbarum
ᗢ 3 grams of technical +98,5%NaOH
ᗢ 3 grams of lab grade Fe(CO)5 from Fluka
Procedure:
500 grams of safrole was put in a 2 liter round bottom flask that was sitting on a heating mantle. Overhead stirring was applied and 3 grams of NaOH and 3 grams of Fe(CO)5 were added. Started heating. Somewhere at 110 degrees C, obvious exothermic reaction kicked in, just like described in Rhodium's isomerization review, and heating was turned off. 15 minutes passed and stirring was turned off and flask was allowed to cool down. When flask was cooled, dark organic mixture was washed with 200 mls 20% acetic acid and then with 200 mls water. Some emulsion formed but that cleared up in about and hour and then organic layer was sepped off with 1 liter separatory funnel. Organic mixture was poured to 2 liter flask, attached claisen still head and liebig condenser with vacuum adapter. Receiving flask was 1 liter round bottom. Vacuum applied and started heating. From 114 C to 118 C at 10 mm vacuum only fraction came over which was almost colourless.
Final yield: 456 grams which means +90% yield. There were some losses during the washes that will be avoided next time and I think +95% yield isn't hard to obtain.