Chlorosulfonic acid → HCID 59759968, Verbindung

HRID 1693138Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1693138
[F:1][C:2]1[CH:14]=[CH:13][C:5]2[S:6][CH:7]=[C:8]([CH2:9][CH:10]([CH3:12])[CH3:11])[C:4]=2[CH:3]=1.[Cl:15][S:16](O)(=[O:18])=[O:17]>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:14]=[CH:13][C:5]2[S:6][C:7]([S:16]([Cl:15])(=[O:18])=[O:17])=[C:8]([CH2:9][CH:10]([CH3:11])[CH3:12])[C:4]=2[CH:3]=1

Komponenten

4

Edukt 2

HCID 24638Chlorosulfonic acidHCID 597599805-Fluoro-3-isobutyl-benzo[b]thiophene

Produkt 1

HCID 59759968HCID 59759968, VerbindungAusbeute 60,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a solution of 5-fluoro-3-isobutyl-benzo[b]thiophene 0.55 g) in chloroform (10 ml) was added chlorosulfonic acid (1.54 g), and the resulting mixture was stirred at rt for 3 h, quenched with ice/water, and extracted with methylene chloride. The organic phases were washed with water and aqueous sodium bicarbonate solution, dried and concentrated. The residue was chromatographed on silica gel using heptane/ethyl acetate as eluent to obtain the title compound (0.49 g) as a colorless oil. MS (EI): 306.8 (M)

Aufarbeitung

  1. customquenched with ice/water
  2. extractionextracted with methylene chloride
  3. washThe organic phases were washed with water and aqueous sodium bicarbonate solution
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-35f862ec1db543008e6a499e0857a2f9
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08158655B2

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