반응 #5600

반응 방정식

2,6-Diphenylphenol

ammonium thiocyanate

→

2'-hydroxy[1,1':3',1"-terphenyl]-5'-yl thiocyanate

용매

methanol

반응 조건

후처리

1. 1
   기타equipped with magnetic stirrer
2. 2
   기타chlorine gas bubbled through the solution for three hours
3. 3
   온도Maintaining the temperature below 10° C., ammonia gas
4. 4
   기타was bubbled through the reaction for 2 hours
5. 5
   workup.ADDITIONThe contents of the flask were then poured
6. 6
   workup.DISTILLATIONinto iced distilled water (250 ml)
7. 7
   여과After filtering
8. 8
   기타the solid was dried in vacuo at 45° C. for 12 hours
9. 9
   기타The title compound was purified by chromatography on silica
10. 10
    기타recrystallized from hexane, m.p. about 104°-106.5° C.

실험 절차

2,6-Diphenylphenol (100.0 g, 0.406 mole) and ammonium thiocyanate (76.99 g, 0.893 mole) were suspended in methanol (150 ml) in a three-necked round bottom flask equipped with magnetic stirrer, thermometer and gas inlet tube. The reaction mixture was cooled to -5° C. in an acetone/ice bath and chlorine gas bubbled through the solution for three hours. Maintaining the temperature below 10° C., ammonia gas was bubbled through the reaction for 2 hours. The contents of the flask were then poured into iced distilled water (250 ml) and allowed to stand for 12 hours in the refrigerator. After filtering, the solid was dried in vacuo at 45° C. for 12 hours. The title compound was purified by chromatography on silica and recrystallized from hexane, m.p. about 104°-106.5° C.

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