Reaktion #155652

ord-c02ce5a6e4d64658935876d0d60677c1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturIce-cooling
  2. 2
    Sonstigeis removed
  3. 3
    Einengenconcentrated under reduced pressure
  4. 4
    Filtrationthe solid is filtered off
  5. 5
    SonstigeThe crude product is purified by flash chromatography over silica gel (dichloromethane)

Vorschrift

An ice-cooled solution of 2.63 ml (35 mmol) of allylamine in 14.2 ml of absolute pyridine and 14.2 ml of absolute THF is admixed dropwise with 5-chloro-thiophene-2-carbonyl chloride (7.61 g, 42 mmol). Ice-cooling is removed and the mixture is stirred at room temperature for 3 h and then concentrated under reduced pressure. The residue is admixed with water and the solid is filtered off. The crude product is purified by flash chromatography over silica gel (dichloromethane).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822458B2uspto-grants-2014_09