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

HRID 356981
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 356981
[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
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

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 0° C. 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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-c3dce65ba56b49ea87ed2ef7b85e228f
Quelldatensatz
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05840736

Notizen zur Reaktion

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