Sodium Azide → 4-Azidomethyl-3-chlorobenzonitrile

HRID 896245

反応式

HRID 896245 の反応式
[Cl:1][C:2]1[CH:9]=[C:8]([C:10]#[N:11])[CH:7]=[CH:6][C:3]=1[CH2:4]Br.[N-:12]=[N+:13]=[N-:14].[Na+]>CN(C=O)C>[Cl:1][C:2]1[CH:9]=[C:8]([C:10]#[N:11])[CH:7]=[CH:6][C:3]=1[CH2:4][N:12]=[N+:13]=[N-:14]

参加物

4

反応物 2

HCID 33557Sodium AzideHCID 130420934-(Bromomethyl)-3-chlorobenzonitrile

生成物 1

HCID 223499744-Azidomethyl-3-chlorobenzonitrile収率 100.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 2-choro-4-cyanobenzyl bromide (6.9 g, 30.0 mmol) in DMF (150 ml), was added sodium azide (2.0 g, 30 mmol) The reaction was stirred overnight at room temperature, and then filtered. The DMF was removed from filtrate in vacuo. The residue was dissolved in EtOAc (300 ml), washed with water (200 ml×3), brine (200 ml×1), dried over sodium sulfate. Removed solvent in vacuo to give 5.8 g of raw 2-choro-4-cyanobenzyl azide.

後処理

  1. filtrationfiltered
  2. customThe DMF was removed from filtrate in vacuo
  3. dissolutionThe residue was dissolved in EtOAc (300 ml)
  4. washwashed with water (200 ml×3), brine (200 ml×1)
  5. dry with materialdried over sodium sulfate

出典と根拠

ORDレコード
ord-c892a0b602544be0bc4b0e6805f9da90
出典データセット
uspto-grants-2005_07
特許番号
US06919347B2

関連ノート

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