1,4-Dibromo-2-nitrobenzene → 4-Bromo-2-nitrobenzonitrile

HRID 1791215ノート

反応式

HRID 1791215 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[C:12]([Cu])#[N:13]>CC(N(C)C)=O.CCOC(C)=O>[Br:8][C:5]1[CH:6]=[CH:7][C:2]([C:12]#[N:13])=[C:3]([N+:9]([O-:11])=[O:10])[CH:4]=1

参加物

5

反応物 2

HCID 770041,4-Dibromo-2-nitrobenzeneHCID 178418546HCID 178418546、化合物

生成物 1

HCID 2925354-Bromo-2-nitrobenzonitrile

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 31374Dimethylacetamide溶媒

実験手順

Stir the mixture of 1,4-dibromo-2-nitro-benzene (3.56 mmol)and CuCN (3.74 mmol) in DMA (4 ml) at 100° C. for 5hours. Cool to room temperature, dilute with EtOAc, filter through celite, wash the organic layer with brine, dry over Na2SO4, and concentrate under vacuum. Purify the residue by flash chromatography (4:1 hexanes/EtOAc) to give 4-bromo-2-nitro-benzonitrile.

後処理

  1. filtrationfilter through celite
  2. washwash the organic layer with brine
  3. dry with materialdry over Na2SO4
  4. concentrationconcentrate under vacuum
  5. customPurify the residue by flash chromatography (4:1 hexanes/EtOAc)

出典と根拠

ORDレコード
ord-4080763d33fc4969b23659b3cd2ed48e
出典データセット
uspto-grants-2006_07
特許番号
US07074799B2

反応ノート

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