Another run done with just a few differences in al/hg time. Also this wacker was run 28 hours instead of 17 on the previous due to cold temps being uncontrollable on the 28 hour run. Pd/cucl2 = 1/4.5 104g alkene/0.82g pdcl2. 95ml Alkene to ~310ml MeOH in a pop bottle at 50 psi down to 30 psi. Total pressure drop between these ranges was 68 psi.
75 ml oil (d=1.175 - 1.176)
11.2 g Al
68 mg Hg
29g 40% hooch + 1 more g added 2 hours after addition (30g)
amalgamated for 25 minutes but amalgamation solvent ~500ml was a litte colder because of ambient temp (~10c)
added 17ml hooch after amalgamated and poured remaing amount into ketone with ~ 175ml MeOH into funnel. Dripped mix in over 25 minutes. Was noticable slower to go exothermic due to ambient temp. additional heat on 2.3 added and stirred full blast. At the 2 hour mark 1 more gram of 40% hooch added. Amalgam ran ~55c. Very little if any reflux drip. Couldn't really see too well into the flask given the opaque flask (from the amalgam). This was intended to run the same time as the previous (4.5 hours). Instead, due to logistical problems it was unable to be run so short. Heat was turned off at the 7 hour mark after drip finished. Ran for another 30 minutes until slightly warm. Dumped grey slurry into 700ml 20% NaOH. But this time no oil fell out. Created an emulsion upon adding toluene probrably because the 20% NaOH was very cold and viscous. Emulsion separated and had to be dealt with using time and patience. 3 extractions totaling 1000ml toluene done over 4 hours. Washed and washed. Acidified with something like 60ml of 31.45% hcl and was still ph 8. Brought it down to 1. Toluene was 5. Cleaned up with acetone (dried this time using 25g MgS04) in 1.1 liter acetone (had about 100ml of toluene added to the acetone too. Resulting yield was 38.5 grams of same goodies as above. MeAm blows the shit out of Nitro. Yields in the part of town have nearly doubled since. Why does this stuff give such bomb-ass yields compared to nitro? I've never had so much. The total of the 2 reactions fill the bottom part of a zip lock bag about 1.5 inches.
