Sodium Azide → 4-Chloro-3-cyanobenzyl azide

HRID 1709663노트

반응식

HRID 1709663 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6]Br)=[CH:4][C:3]=1[C:10]#[N:11].[N-:12]=[N+:13]=[N-:14].[Na+]>C(O)C>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][N:12]=[N+:13]=[N-:14])=[CH:4][C:3]=1[C:10]#[N:11]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 140330355-(Bromomethyl)-2-chlorobenzonitrile

생성물 1

HCID 230362384-Chloro-3-cyanobenzyl azide수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A stirred mixture of 4-chloro-3-cyanobenzyl bromide (3.0 g, 13 mmol) and sodium azide (1.26 g, 19.4 mmol) was refluxed 5 hours in absolute ethanol (30 mL). The mixture was kept 18 hours at ambient temperature, filtered, and the filtrate was evaporated under vacuum. The residue was triturated with diethyl ether, filtered, and evaporated to provide 2.45 g (98%) liquid 4-chloro-3-cyanobenzyl azide; I.R. (neat): 2240, 2100 cm1.

후처리

  1. filtrationfiltered
  2. customthe filtrate was evaporated under vacuum
  3. customThe residue was triturated with diethyl ether
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-f35ccbb7e93e459ab59c2fdf8f278e0e
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04950673

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