Reaktion #4781

Reaktionsgleichung

ammonium thiocyanate

benzoyl chloride

chloroform

5-aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine

→

5-(3-benzoylthioureidomethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine

Ausbeute 81.0%

Lösungsmittel

acetone

water

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 2 hours
2. 2
   TemperaturAfter refluxing for 2 hours
3. 3
   SonstigeThe organic layer was separated
4. 4
   Waschenwashed with saturated aqueous sodium chloride
5. 5
   Trocknendried over magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off
7. 7
   Sonstigethe resulting crystal was recrystallized from diisopropyl ether

Vorschrift

A mixture of ammonium thiocyanate (0.25 g) and benzoyl chloride (0.41 g) in acetone (20 ml) was refluxed for 2 hours, and 5-aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (0.9 g) in acetone (5 ml) was added thereto. After refluxing for 2 hours, the reaction mixture was poured into a mixture of chloroform (100 ml) and water (50 ml). The organic layer was separated, washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The solvent was distilled off and the resulting crystal was recrystallized from diisopropyl ether to give 5-(3-benzoylthioureidomethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (1.1 g).

Quelle