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

HRID 280640노트

반응식

HRID 280640 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 136496614-(4-Chlorobenzoyl)-3-chlorobenzyl azide수율 106.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ee83f3216d8e4f2f9e9b60dabba91e4f
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04590201

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