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4-Chlorobenzoyl chloride → 4-Chloro-N-[3-(1H-imidazol-1-yl)propyl]benzamide

HRID 565419
ノート
印刷プレビュー

反応式

HRID 565419 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[CH:9]=[CH:8][N:7]=[CH:6]1.C(N(C(C)C)CC)(C)C.[Cl:19][C:20]1[CH:28]=[CH:27][C:23]([C:24](Cl)=[O:25])=[CH:22][CH:21]=1>C(Cl)Cl>[N:5]1([CH2:4][CH2:3][CH2:2][NH:1][C:24](=[O:25])[C:23]2[CH:27]=[CH:28][C:20]([Cl:19])=[CH:21][CH:22]=2)[CH:9]=[CH:8][N:7]=[CH:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 85014-Chlorobenzoyl chlorideHCID 787361H-Imidazole-1-propanamineHCID 81531Diisopropylethylamine

生成物 1

HCID 28426644-Chloro-N-[3-(1H-imidazol-1-yl)propyl]benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 1-(3-amino-propyl)imidazole (2.1 g, 16.8 mmol), diisopropyl-ethylamine (3.5 mL, 20.0 mmol) and 4-N,N-dimethyl-aminopyridine (200 mg, 1.7 mmol) in methylene chloride (15 mL) at 0C was added dropwise 4-chlorobenzoyl-chloride (2.1 mL, 16.8 mmol). The reaction was then allowed to warm to room temperature. After 5 hours, the reaction was diluted with methylene chloride, washed with 1N sodium hydroxide, brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to provide a white solid. This material was washed with diethyl ether to provide N-(3-imidazol-1-yl-propyl)-4-chlorobenzamide. To a slurry of the above amide (1.58 g, 6.0 mmol) in tetrahydrofuran (30 mL) was slowly added lithium aluminum hydride (456 mg, 12.0 mmol) upon which the reaction became exothermic. The mixture was heated to 80° C., stirred for 1 hr, cooled to 0° C. and quenched by addition of water (0.5 mL), 15% sodium hydroxide (0.5 mL) and an additional 1.5 mL of water. The reaction was diluted with ethyl acetate, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to provide compound 20.

後処理

  1. washwashed with 1N sodium hydroxide, brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto provide a white solid
  6. washThis material was washed with diethyl ether

出典と根拠

ORDレコード
ord-7108b0f8a82d406db978286960bdb063
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06172086B2

反応ノート

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