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

HRID 484182

反応式

HRID 484182 の反応式
[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

参加物

4

反応物 2

HCID 15666Ammonium thiocyanateHCID 755122,6-Diphenylphenol

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
-5 °C

実験手順

2,6,-Diphenylphenol (100.0 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 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.

後処理

  1. customequipped with magnetic stirrer
  2. customchlorine gas 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. about 104°-106.5° C.

出典と根拠

ORDレコード
ord-19e87480ec9a49a4b9cc16e0d5d7aa4d
出典データセット
uspto-grants-1993_07
特許番号
US05229421

関連ノート

読み込み中…