반응 #521528

반응 방정식

N-dichloromethylene 4-cyclohexylaniline

1,3-diaminopropane

triethylamine

→

2-(4-cyclohexylphenyl)imino-hexahydropyrimidine

용매

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   여과after which the reaction mixture is filtered
2. 2
   온도while warm
3. 3
   workup.DISTILLATIONAfter distilling off the solvent the residue
4. 4
   세척successively washed with 2 N sodium hydroxide solution and water
5. 5
   건조The ether layer is dried
6. 6
   기타evaporated
7. 7
   기타after which the residue is recrystallised from acetonitrile

실험 절차

A solution of 2.6 g of N-dichloromethylene 4-cyclohexylaniline in 40 ml of acetonitrile is added dropwise to a solution of 1 ml of 1,3-diaminopropane in 20 ml of acetonitrile in 15 minutes at room temperature. After the addition of 1 ml of triethylamine, the solution is stirred for 1 hour at room temperature, after which the reaction mixture is filtered while warm. After distilling off the solvent the residue is taken up in ether and successively washed with 2 N sodium hydroxide solution and water. The ether layer is dried and evaporated, after which the residue is recrystallised from acetonitrile. The resulting 2-(4-cyclohexylphenyl)imino-hexahydropyrimidine has a melting point of 180°-182° C.

출처