3-Methylthiophene → 3-Methylthiophene-2-sulfonyl chloride

HRID 1730067

Reaktionsgleichung

Reaktionsgleichung von HRID 1730067
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][CH:3]=1.[Cl:7][S:8](O)(=[O:10])=[O:9]>C(Cl)(Cl)Cl.C(=O)(O)[O-].[Na+]>[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[S:8]([Cl:7])(=[O:10])=[O:9]

Komponenten

5

Edukt 2

HCID 120243-MethylthiopheneHCID 24638Chlorosulfonic acid

Produkt 1

HCID 134257133-Methylthiophene-2-sulfonyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 516892Sodium BicarbonateLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

A 49-g (0.5 mol) sample of 3-methylthiophene was added in small portions to a cooled solution (-20° C) of 128 g (1 mol) chlorosulfonic acid in 250 cc chloroform. After the addition was completed, the reaction mixture was allowed to warm to about 25° C and then heated at reflux for 30 minutes. The reaction mixture was then diluted with ice water and neutralized with aqueous sodium bicarbonate solution. The organic layer was separated, dried over magnesium sulfate and evaporated to give 30 g of 3-methyl-2-thienylsulfonyl chloride.

Aufarbeitung

  1. additionAfter the addition
  2. temperatureheated
  3. temperatureat reflux for 30 minutes
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-daee733669fe41d397471f0f084a84c8
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03991081

Verknüpfte Notizen

Wird geladen…