Reaktion #11382

Reaktionsgleichung

3-amino-2-cyclohexylaminopyridine

ethoxycarbonyl isothiocyanate

dipropylamine

→

Ethyl {[2-(cyclohexylamino)-3-pyridyl]imino}(diethylamino)methylcarbamate

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe ice bath is removed
2. 2
   workup.ADDITIONAfter diluting the solution
3. 3
   Filtrationwith 100 ml of ethyl acetate, filtration
4. 4
   Sonstigethe solvents are evaporated off under reduced pressure
5. 5
   SonstigeThe resulting crude product is then recrystallised from acetonitrile

Vorschrift

A mixture of 0.02 mol (3.82 g) of 3-amino-2-cyclohexylaminopyridine from Preparation 1 and 0.02 mol of ethoxycarbonyl isothiocyanate is stirred in 50 ml of DMF at ambient temperature for 3 hours. The solution is then cooled to 0° C., and 0.05 mol of dipropylamine and then 0.02 mol of mercuric chloride are added in succession. After 15 minutes, the ice bath is removed and the solution is stirred at ambient temperature for 4 hours. After diluting the solution with 100 ml of ethyl acetate, filtration is carried out over Celite and the solvents are evaporated off under reduced pressure. The resulting crude product is then recrystallised from acetonitrile.

Quelle