反応 #11382

反応方程式

3-amino-2-cyclohexylaminopyridine

ethoxycarbonyl isothiocyanate

dipropylamine

→

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

溶媒

DMF

反応条件

後処理

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

実験手順

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.

出典