Potassium azide → 4-(4-Chlorobenzoyl)-3-chlorobenzyl azide

HRID 280640ノート

反応式

HRID 280640 の反応式
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:15]=[CH:14][C:11]([CH2:12]Br)=[CH:10][C:9]=2[Cl:16])=[O:7])=[CH:4][CH:3]=1.[N-:19]=[N+:20]=[N-:21].[K+]>C(O)C>[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:15]=[CH:14][C:11]([CH2:12][N:19]=[N+:20]=[N-:21])=[CH:10][C:9]=2[Cl:16])=[O:7])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 10290740Potassium azideHCID 136496544-(4-Chlorobenzoyl)-3-chlorobenzyl bromide

生成物 1

HCID 136496614-(4-Chlorobenzoyl)-3-chlorobenzyl azide収率 106.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred suspension of 4-(4-chlorobenzoyl)-3-chlorobenzyl bromide (1.60 g, 4.65 mmol) and potassium azide (0.715 g, 8.81 mmol) in ethanol (15 ml) was refluxed 5 hours, cooled to ambient temperature, and stirred 16 hours. The solids were filtered and washed twice with ethanol. The combined filtrate and washes were evaporated under vacuum, diluted with diethyl ether (40 ml), filtered, and evaporated under vacuum to provide 1.51 g (106% of theory) of 4-(4-chlorobenzoyl)-3-chlorobenzyl azide, m.p. 33°-33.5° C., suitable for subsequent reaction.

後処理

  1. temperaturewas refluxed 5 hours
  2. filtrationThe solids were filtered
  3. washwashed twice with ethanol
  4. customThe combined filtrate and washes were evaporated under vacuum
  5. additiondiluted with diethyl ether (40 ml)
  6. filtrationfiltered
  7. customevaporated under vacuum

出典と根拠

ORDレコード
ord-ee83f3216d8e4f2f9e9b60dabba91e4f
出典データセット
uspto-grants-1986_05
特許番号
US04590201

反応ノート

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