Here are the notes that were kept during the rxn antibody discussed above (please note that an american thermometer was used during rxn)
1l heavy walled filterflask in a waterbath fixed with a 1.25" victor tire valve, was charged w/0.5g PdCl2, 2.5g CuCl2, 100ml 99%IPA, 2.5 " egg shaped stirbar. Stirred overnight.
9:30: flask was charged with 50g safrole (0.28 moles), pressurized to 50psi, set stirrer on high, cooled bath from 61deg F->55deg F over 0.5hr
10:00: Stopped stirring, pressure had dropped to 40psi, opened flask charged with 3.5ml dH2O, resealed flask and repressurize to 50psi.
10:30: Pressure had dropped to 38psi bath temp had risen to 62Deg F, added two more ice cubes to bath, repressurize to 50psi.
11:10: Pressure had dropped to 43psi bath temp had risen to 66Deg F, added three more ice cubes to bath, repressurize to 50psi.
11:40: Pressure had dropped to 45psi bath temp had risen to 66Deg F, added three more ice cubes to bath(bath tempo dropped to 56F), repressurize to 50psi.
12:20: Pressure had dropped to 44psi bath temp had risen to 64Deg F, added two more ice cubes to bath, repressurize to 50psi.
12:55: Pressure had dropped to 45psi. Stirring was stopped.
Total pressure drops 45psi or 3atm. In this flask with the reactants there remained 1.1litre headroom.
1l of Oxygen @1atm =1.42g
3.3l Oxygen @ 3atm =4.686g
0.2947moles of oxygen was consumed by reaction, a slight molar excess relative to safrole.
IPA was distilled at 45degC under medium vac, the remaining oil was passed through .25" 50mesh silica sand in a vacuum filtration set-up to recover catalyst.
Stirred filtrate with 200ml dH2O and 20ml 31% HCl for 15 minutes. Red oil that fell out was separated and the aqueous layer is extracted with 20ml DCM which is pooled w/ previous extract and placed in a 250ml rb flask in an oil bath, DCM is stripped off @ 760ttorr.
High Vac attached and applied
4mls of forerun are collected and discarded
30mls of safrole collected at 102-104 deg C
7mls ketone collected at 104-138 deg C
bit of polymerized crud in flask
Notes: the 2nd two fractions were tested with sodium metabisulfite 1ml each. The 3rd fraction crystallized immediately in the normal fashion, the 2nd fraction initially did nothing, but upon vigourous shaking finally began become turbid forming fluffy cystals over 1hour period at RT. (Crystals unlike any previously witnessed in similar rxns)
The 2nd fraction was reacted in a MM nitro Al/Hg, used the Ritter work-up, pregassed toulene was added to the washed and driied toulene extract until ph5 is reached. Nothing An hour later additional pregassed toulene added bringing PH down to 2 yield=0.0g+ONE PISSED OFF BEE
Total time elapsed 11.5hours.
So there it is, flames welcome, Placebo?
Jimi loves ya