Hydrochloric Acid → 4-(4-Iodophenyl)benzonitrile

HRID 2372978

反応式

HRID 2372978 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 13930054-(4-Iodophenyl)benzonitrile収率 86.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
200 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-416499616194444f888a6cad8972cf0f
出典データセット
uspto-grants-1992_03
特許番号
US05101048

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