Foreword
Ladies and gentlemen!
Let me proudly introduce to you another story from Zealot’s dream collection.
While there’s 6 steps in the synthesis, its longitude is explained by the fact that all the precursors and even some reagents are made from scratch, employing user-friendly techniques and equipment (in fact, a need for vacuum is mentioned only once, and even that is for the removal of solvent); as well as only easy-to-get reactants.
Study please Russian
Most difficult 1 step.
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Phenylaminoacotonitrile HCl
Dissolve 30 g KCN and 25 NH4Cl in possible small quantity of water. Then add 50 g benzaldehyde
and methanol that all aldehyde has passed in a solution.
Very soon there is a turbidity rm, and in half an hour is formed amuls.
Through 2-3 ÷ the reaction comes to an end — at the bottom flask the heavy yellow oil is allocated.
Product of reaction take by an ether, wash out by water and after evaporation ether, add by 10% hydrochloric acid.
Insignificant part of oil, not dissolve in a hydrochloric acid, extracted by an ether.From a sour water solution at slow evaporation the well formed crystals HCl.
Them separate, filtrat concentrated by evaporation and receive a little more crystals.Yield 45-53 g.
Step 2
N-Phenylacetonitrylurea
50 g Phenylaminoacotonitrile dissolve in 300 Ml water. Heat to 70-80 and small portions add to a mix 20 g (19,4g - teor.) cianat sodium.After 4-5 hours of continuous heating the mix We haven two layers.After stop within night at room temperature the product of reaction crystallizes. Separated on a funnel in vacuum, wash out by ice water and probably dry on a funnel. For clearing the product is possible recristalisation from ethylacetat or butylacetat.
Yield 47g (91 % teor.).