반응 #65599

반응 방정식

3-chloro-4-(4-chloro-1-naphthoxy)-2,5-dimethylaniline

2,6-difluorobenzoyl isocyanate

→

1-[3-chloro-4-(4-chloro-1-naphthoxy)-2,5-dimethylphenyl]-3-(2.6-difluorobenzoyl)urea

수율 62.3%

용매

toluene

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONwas slowly added a solution
2. 2
   온도was cooled to room temperature
3. 3
   기타placed in an ice bath
4. 4
   여과filtered through a Buchner funnel
5. 5
   기타The collected solid was dried under a vacuum at a temperature of 50° C.

실험 절차

Into a solution containing 3.0 grams (9.0 mmol) of 3-chloro-4-(4-chloro-1-naphthoxy)-2,5-dimethylaniline prepared in Part B of Example I in 25 milliliters of toluene which solution was warmed to a temperature of 50° C. and placed under a nitrogen atmosphere was slowly added a solution containing 2.5 grams (13.5 mmol) of 2,6-difluorobenzoyl isocyanate in 5 milliters of toluene. After stirring for one hour at a temperature of 50° C. the reaction mixture was cooled to room temperature, placed in an ice bath, and filtered through a Buchner funnel. The collected solid was dried under a vacuum at a temperature of 50° C. to afford 2.89 grams of 1-[3-chloro-4-(4-chloro-1-naphthoxy)-2,5-dimethylphenyl]-3-(2.6-difluorobenzoyl)urea as a white powder havin a melting point of 187° C. Elemental analysis of the white powder indicated the following:

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