Sodium Azide → 4-Azidomethyl-3-chlorobenzonitrile

HRID 896245

반응식

HRID 896245 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 223499744-Azidomethyl-3-chlorobenzonitrile수율 100.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c892a0b602544be0bc4b0e6805f9da90
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06919347B2

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