Sodium Azide → 4-Chloro-3-cyanobenzyl azide

HRID 1194717ノート

反応式

HRID 1194717 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 230362384-Chloro-3-cyanobenzyl azide収率 98%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-2d9efaf094644f2fb1db6891b7fc2a98
出典データセット
uspto-grants-1989_03
特許番号
US04816469

反応ノート

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