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Pyridine → 5-Chloro-3-iodo-1H-pyrrolo[2,3-b]pyridine

HRID 509921
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 509921
[Cl:1][C:2]1[CH:3]=[C:4]2[CH:10]=[CH:9][NH:8][C:5]2=[N:6][CH:7]=1.N1C=CC=CC=1.[I:17]Cl>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:10]([I:17])=[CH:9][NH:8][C:5]2=[N:6][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 24640Iodine chlorideHCID 242292135-Chloro-1H-pyrrolo[2,3-b]pyridine

Produkt 1

HCID 242292205-Chloro-3-iodo-1H-pyrrolo[2,3-b]pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 5-chloro-1H-pyrrolo[2,3-b]pyridine (1, 15.00 g, 98.31 mmol) in 300 mL of dichloromethane under nitrogen, pyridine (7.951 mL, 98.31 mmol) and iodine monochloride (110 mL, 1.0 M in dichloromethane, 110 mmol) were added slowly over 20 minutes. The reaction was stirred at room temperature for 2 hours, then quenched with 100 mL of 1 M aqueous sodium thiosulfate pentahydrate. The layers were separated, solids collected from the aqueous layer by filtration and combined with the organic layer. The aqueous layer was extracted with ethyl acetate, organic layers were combined and washed with brine, then concentrated under vacuum. The resulting solid was washed with 20% ethyl acetate in hexane to provide the desired compound. 5-fluoro-3-iodo-1H-pyrrolo[2,3-b]pyridine is prepared similarly from 5-fluoro-1H-pyrrolo[2,3-b]pyridine.

Aufarbeitung

  1. customquenched with 100 mL of 1 M aqueous sodium thiosulfate pentahydrate
  2. customThe layers were separated
  3. filtrationsolids collected from the aqueous layer by filtration
  4. extractionThe aqueous layer was extracted with ethyl acetate, organic layers
  5. washwashed with brine
  6. concentrationconcentrated under vacuum
  7. washThe resulting solid was washed with 20% ethyl acetate in hexane

Quellen und Nachweise

ORD-Eintrag
ord-8061cae26e264945a3468a0ed4a26165
Quelldatensatz
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09096593B2

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