Reaktion #72534

Reaktionsgleichung

compound

2,2,2-Trichloro-1-(1H-pyrrol-2-yl)ethanone

AlCl3

dichloro-methoxy-methane

→

title product

5-(Trichloroacetyl)-1H-pyrrole-3-carbaldehyde

Lösungsmittel

DCM nitromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeat −30° C.
2. 2
   ExtraktionThe aqueous phase is extracted with AcOEt
3. 3
   WaschenThe organic phase is washed with saturated aqueous NaCl solution
4. 4
   Trocknendried over sodium sulphate
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated to dryness

Vorschrift

To a solution of the compound obtained in Step A (87 mmoles) and AlCl3 in a DCM/nitromethane mixture (80 ml/80 ml) there is added, dropwise, at −30° C., dichloro-methoxy-methane (130.5 mmoles). After stirring for two hours, the reaction mixture is poured into 800 ml of ice-cold water. The aqueous phase is extracted with AcOEt, and then the organic phases are combined. The organic phase is washed with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness to yield the title product (brown crystals), which is used directly in the next Step.

Quelle