反応 #72534

反応方程式

compound

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

AlCl3

dichloro-methoxy-methane

→

title product

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

溶媒

DCM nitromethane

反応条件

後処理

1. 1
   その他at −30° C.
2. 2
   抽出The aqueous phase is extracted with AcOEt
3. 3
   洗浄The organic phase is washed with saturated aqueous NaCl solution
4. 4
   乾燥dried over sodium sulphate
5. 5
   ろ過filtered
6. 6
   その他evaporated to dryness

実験手順

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.

出典