Pyridinium chloride → HCID 13290010, Verbindung

HRID 370942Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 370942
[Cl:1][C:2]1[C:3]([O:14]C)=[CH:4][C:5]2[CH:9]=[C:8]([CH2:10][CH3:11])[S:7][C:6]=2[C:12]=1[Cl:13].Cl.N1C=CC=CC=1>>[Cl:1][C:2]1[C:3]([OH:14])=[CH:4][C:5]2[CH:9]=[C:8]([CH2:10][CH3:11])[S:7][C:6]=2[C:12]=1[Cl:13]

Komponenten

3

Edukt 2

HCID 10176127Pyridinium chlorideHCID 13290009HCID 13290009, Verbindung

Produkt 1

HCID 13290010HCID 13290010, VerbindungAusbeute 73,7 %

Versuchsvorschrift

A mixture of 2.15 g of 6,7-dichloro-2-ethyl-5-methoxybenzo[b]thiophene and 15 g of pyridine hydrochloride is stirred at 170°-180° for 90 min. The mixture is cooled, triturated with water and extracted three times with dichloromethane. The combined organic extracts are washed with water, dried over anhydrous magnesium sulfate and concentrated in vacuo to an oily residue. Purification by column chromatography (silica gel-etherpentane 50:50) affords 1.5 g of 6,7-dichloro-2-ethyl-5-hydroxybenzo[b]thiophene as off-white crystals, mp 69°-70°.

Aufarbeitung

  1. temperatureThe mixture is cooled
  2. customtriturated with water
  3. extractionextracted three times with dichloromethane
  4. washThe combined organic extracts are washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo to an oily residue
  7. customPurification by column chromatography (silica gel-etherpentane 50:50)

Quellen und Nachweise

ORD-Eintrag
ord-4181b812fa074a819138e9d868166665
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04528399

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