I made electrosynthesis piperidine of pyridine.
This expedient is tested many times and works very good!
See:
Post 366798 (missing)
(fallen_Angel: "Ýëåêòðîñèíòåç ïèïåðèäèíà", Russian HyperLab)The lead plate are made of clean lead.
The diaphragm is made of glass tissue and is glued by a liquid silica glass. It is little bit more, than lead plate. Then the diaphragm is acidized and is washed by water. At pouring in not ¸ of water, the water should drip very much slowly, 1-5 drips one minute
The plates wash by hydrogen nitrate.
On 1 liter of electrolyte for lead accumulators takes 100 mls of pyridine, the plates alight and the current is included. A current intensity 10-15 amperes of \100 centimeters2, (+) and (-) change places, and then in 5 minutes again vary. It is necessary for an enhancement of activity of plates. In diaphragm the plate is (+). After a gear transmission 800 amperes*clocks on each 100 mls of pyridine, mass evolves into a flask and is neutralized NaOH up to pH~11-12 of response. Then the equal water volume is added and is distilled off 500-700 mls on taken 100 mls of pyridine. Then distillate title concentrated HCL strictly up to pH=9-10 (decolourization of phenolphthalein), and distil off unreacted pyridine. A solution volatilize up to volume 200 mls on each 1 of the mol spent acid, and at once will utillize in synthesis PCP (add 1 mol KCN and 0,9 mol of cyclohexanone on 1 mol of spent acid). It is possible to bleed and clean chloride of piperidine, vapouring a solution.
Yield of piperidine 50 %, from 1 liter of pyridine - > 0,6 liters of piperidine (6 mol of chloride).
Features:
1. The lead should be very clean.
2. All reagents do not owe ñîäåðæàòüäàæå a tramp iron or other metals.
3. The reactionary vessel should be chilled - to put in a basin with cool water.
You can use electrical power unit for the accumulator or device for welding for this synthesis - it is depends on quantity of materials, which one you will use.
Fallen_Angel
