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Sodium Azide → 3-(4-Chlorobenzoyl)-benzyl azide

HRID 280637
ノート
印刷プレビュー

反応式

HRID 280637 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:9]=[C:10]([CH:13]=[CH:14][CH:15]=2)[CH2:11]Br)=[O:7])=[CH:4][CH:3]=1.[N-:18]=[N+:19]=[N-:20].[Na+]>C(O)C>[Cl:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:9]=[C:10]([CH:13]=[CH:14][CH:15]=2)[CH2:11][N:18]=[N+:19]=[N-:20])=[O:7])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 33557Sodium AzideHCID 136496533-(4-Chlorobenzoyl)benzyl bromide

生成物 1

HCID 136496603-(4-Chlorobenzoyl)-benzyl azide収率 100.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3-(4-chlorobenzoyl)benzyl bromide (4.2 g, 13.6 mmol) and sodium azide (1.32 g, 20.3 mmol) in ethanol (40 ml) was refluxed for 5 hours, cooled to ambient temperature, and kept 16 hours. The mixture was filtered and the solids were washed twice with ethanol. The combined filtrate and washes were evaporated to dryness under vacuum and the residue was treated with diethyl ether and filtered. The filtrate was evaporated to dryness under vacuum and dried to provide 3.7 g (100%) of 3-(4-chlorobenzoyl)-benzyl azide, m.p. 43°-45° C.

後処理

  1. temperaturewas refluxed for 5 hours
  2. filtrationThe mixture was filtered
  3. washthe solids were washed twice with ethanol
  4. customThe combined filtrate and washes were evaporated to dryness under vacuum
  5. additionthe residue was treated with diethyl ether
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness under vacuum
  8. customdried

出典と根拠

ORDレコード
ord-797ab928d8754b319797ffa3ce390464
出典データセット
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04590201

反応ノート

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