Hydrochloric Acid → 4-(4-Iodophenyl)benzonitrile

HRID 2372978

반응식

HRID 2372978 반응식
I[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([I:14])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[Hg](C#N)[C:16]#[N:17].N1C=CC=CC=1.Cl>CN(C)C=O>[I:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]2[CH:6]=[CH:7][C:2]([C:16]#[N:17])=[CH:3][CH:4]=2)=[CH:9][CH:10]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 11591Mercuric cyanideHCID 763484,4'-Diiodo-1,1'-biphenyl

생성물 1

HCID 13930054-(4-Iodophenyl)benzonitrile수율 86.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
200 °C

실험 절차

A mixture of 15 g (33.2.10-3 mol) of 4,4'-diiodo-1,1'-biphenyl, 3.13 g (34.9.10-3 mol) of mercuric cyanide and 2.75 g (34.9.10-3 mol) of pyridine is heated at 200° C. for 15 minutes and 6 ml of dimethylformamide are then added to the mixture. After cooling, the reaction medium is hydrolyzed with a 1N aqueous solution of hydrochloric acid. The expected product is extracted with ethyl acetate. The organic phase obtained is washed with water until the pH of the washings is neutral, dried over magnesium sulfate and evaporated under vacuum. 3.28 g (yield: 33%) of a yellow solid are obtained after purification by flash chromatography using a chloroform/toluene mixture (1/1 v/v) as the eluent.

후처리

  1. temperatureAfter cooling
  2. extractionThe expected product is extracted with ethyl acetate
  3. customThe organic phase obtained
  4. washis washed with water until the pH of the washings
  5. dry with materialdried over magnesium sulfate
  6. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-416499616194444f888a6cad8972cf0f
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05101048

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