반응 #72534

반응 방정식

compound

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

AlCl3

dichloro-methoxy-methane

→

title product

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

용매

DCM nitromethane

반응 조건

후처리

1. 1
   기타at −30° C.
2. 2
   추출The aqueous phase is extracted with AcOEt
3. 3
   세척The organic phase is washed with saturated aqueous NaCl solution
4. 4
   건조dried over sodium sulphate
5. 5
   여과filtered
6. 6
   기타evaporated to dryness

실험 절차

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.

출처