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Water → 4-Chloro-5-ethyl-2-thiophenecarboxaldehyde

HRID 221055
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 221055
[CH2:1]([C:3]1[S:7][C:6]([CH:8]=[O:9])=[CH:5][CH:4]=1)[CH3:2].[Cl:10]N1C(=O)CCC1=O.O>CN(C)C=O>[Cl:10][C:4]1[CH:5]=[C:6]([CH:8]=[O:9])[S:7][C:3]=1[CH2:1][CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 962WaterHCID 31398Chlorosuccinimide2×HCID 1698305-Ethyl-2-thiophenecarboxaldehyde

Produkt 1

HCID 838743164-Chloro-5-ethyl-2-thiophenecarboxaldehydeAusbeute 41,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 5-ethyl-2-thiophenecarboxaldehyde (6.0 g) in N,N-dimethylformamide (60 ml) was added N-chlorosuccinimide (8.57 g), and the mixture was stirred at room temperature for 2 hours, and subsequently stirred under heating at 60° C. for 2 hours. N-chlorosuccinimide (4.00 g) was further added thereto, and the mixture was further stirred under heating at 60° C. for 2 hours. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate, washed with brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=33:1) to give 4-chloro-5-ethyl-2-thiophenecarboxaldehyde (3.1 g) as colorless oil. (2) The above 4-chloro-5-ethyl-2-thiophenecarboxaldehyde was treated in a manner similar to Reference Example 1 to give 3-bromo-1-(4-chloro-5-ethyl-2-thienylmethyl)benzene as yellow oil. APCI-Mass m/Z 347/349 (M+H+MeOH).

Aufarbeitung

  1. stirringsubsequently stirred
  2. temperatureunder heating at 60° C. for 2 hours
  3. stirringthe mixture was further stirred
  4. temperatureunder heating at 60° C. for 2 hours
  5. extractionthe mixture was extracted with ethyl acetate
  6. washwashed with brine
  7. dry with materialdried over sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=33:1)

Quellen und Nachweise

ORD-Eintrag
ord-013185b1457e450d8cb505bf2cd60f3f
Quelldatensatz
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08202984B2

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