3-Bromo-7-methyl-1-benzothiophene → 3-Cyano-7-methylbenzo[b]thiophene

HRID 649013ノート

反応式

HRID 649013 の反応式
Br[C:2]1[C:3]2[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:4]=2[S:5][CH:6]=1.[C:12]([Cu])#[N:13]>N1C=CC=CC=1>[C:12]([C:2]1[C:3]2[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:4]=2[S:5][CH:6]=1)#[N:13]

参加物

4

反応物 2

HCID 6150893-Bromo-7-methyl-1-benzothiopheneHCID 178418546HCID 178418546、化合物

生成物 1

HCID 147804933-Cyano-7-methylbenzo[b]thiophene

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

3 g of 3-bromo-7-methylbenzo[b]thiophene and 1.1 g CuCN are dissolved in dry pyridine and heated at 220° in an autoclave for 12 hours. The mixture is cooled, concentrated, the residue partitioned between dichloromethane and dilute HCl and the organic phase washed, dried and concentrated. Chromatography of the residue over silica gel (toluene) yields the title compound as pale-yellow crystals. M.p.=82°-84°.

後処理

  1. temperatureheated at 220° in an autoclave for 12 hours
  2. temperatureThe mixture is cooled
  3. concentrationconcentrated
  4. customthe residue partitioned between dichloromethane and dilute HCl
  5. washthe organic phase washed
  6. customdried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-c90280854a7b4e6fafb5bea2ad624009
出典データセット
uspto-grants-1988_04
特許番号
US04737516

反応ノート

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