Reaktion #69360

ord-d34cb3ece78144f5b8c257a05ed29ffc

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: US08530505B2uspto-grants-2013_09