Sodium Azide → 4-Chloro-3-cyanobenzyl azide
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
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
- filtrationfiltered
- customthe filtrate was evaporated under vacuum
- customThe residue was triturated with diethyl ether
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-3c891f33b847442097777ea209d70180
- 出典データセット
- uspto-grants-1988_01
- 特許番号
- US04721791
反応ノート
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