반응 #63967

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4-(4-chlorophenoxy)aniline

trichloromethylchloroformate

3-(4-chlorophenyl)-4-phenylpyrazoline

→

3-(4-chlorophenyl)-N-[4-(4-chlorophenoxy)phenyl]-4-phenylpyrazoline-1-carboxamide

수율 53.9%

용매

diethyl ether

toluene

toluene

diethyl ether

반응 조건

후처리

1. 1
   workup.ADDITIONAfter complete addition
2. 2
   온도This mixture was cooled to room temperature
3. 3
   기타the solvent evaporated under reduced pressure
4. 4
   기타to leave a residue
5. 5
   기타The solvent was evaporated from the mixture

실험 절차

To a stirred solution of 0.75 g (0.0034 mole) 4-(4-chlorophenoxy)aniline in 25 mL of toluene was added dropwise a solution of 0.43 mL (0.0036 mole) trichloromethylchloroformate in 20 mL of toluene. After complete addition, the mixture was heated at 85° C. for three hours. This mixture was cooled to room temperature and the solvent evaporated under reduced pressure to leave a residue. The residue was dissolved in 25 mL of diethyl ether. This solution was added dropwise to a stirred slurry of 1.0 g (0.0034 mole) of 3-(4-chlorophenyl)-4-phenylpyrazoline in diethyl ether. Three drops of triethylamine were added and the mixture was stirred at room temperature for two days. The solvent was evaporated from the mixture to yield 0.92 g of 3-(4-chlorophenyl)-N-[4-(4-chlorophenoxy)phenyl]-4-phenylpyrazoline-1-carboxamide (mp 158°-161° C.).

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