Ammonium thiocyanate → 2'-Hydroxy[1,1':3',1"-terphenyl]5'-yl thiocyanate

HRID 275417

반응식

HRID 275417 반응식
[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:8]=2[OH:19])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[S-:20][C:21]#[N:22].[NH4+]>CO>[OH:19][C:8]1[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:12][C:11]([S:20][C:21]#[N:22])=[CH:10][C:9]=1[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

4

반응물 2

HCID 15666Ammonium thiocyanateHCID 755122,6-Diphenylphenol

생성물 1

HCID 138229422'-Hydroxy[1,1':3',1"-terphenyl]5'-yl thiocyanate

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
-5 °C

실험 절차

2,6-Diphenylphenol (100 g, 0.406 mole) and ammonium thiocyanate (67.99 g, 0.893 mole) were suspended in methanol (150 ml) in a three necked round bottom flask equipped with magnetic stirrer, thermometer and bubbler. The reaction mixture was cooled to -5° C. in an acetone/ice bath and chlorine gas was 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. 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. ca. 104°-106.5° C.

후처리

  1. customequipped with magnetic stirrer
  2. customchlorine gas was bubbled through the solution for three hours
  3. temperatureMaintaining the temperature below 10° C., ammonia gas
  4. customwas bubbled through the reaction for 2 hours
  5. additionThe contents of the flask were then poured
  6. distillationinto iced distilled water (250 ml)
  7. filtrationAfter filtering
  8. customthe solid was dried in vacuo at 45° C. for 12 hours
  9. customThe title compound was purified by chromatography on silica
  10. customrecrystallized from hexane, m.p. ca. 104°-106.5° C.

출처 및 근거

ORD 기록
ord-7ca2a338bf574f66996d17a247574eb3
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393764

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