Flash Chromatography Note #61: Isolation of 3-Nitro-4-ethoxybenzaldehyde

Buchi Flash Chromatography Sepacore System

Buchi Flash Chromatography Sepacore System

This flash chromatography short note describes a simple and fast procedue for the isolation of 3-Nitro-4-ethoxybenzaldehyde from a synthesis mixture. Visit our Sepacore Flash Chromatography Applicationssection to download this short note and review all our other available application studies.

Sepacore Configuration:
Cartridge 12 x 150mm, prepacked with silica gel 60, 40 – 63 μm
2 Pump Modules C-605
Fraction Collector C-660
Control-Unit C-620 with SepacoreControl software
UV Photometer C-635

First Separation Conditions:
Eluent: n-hexane with 25 / 50 / 75% ethyl acetate (%B), step gradient
Flow rate: 10ml/min
Sample: 0.5 g crude mixture, dissolved in n-hexane/ethyl acetate 75:25
Injection volume: 1ml

Under these conditions the impurity with the shortest elution time cannot be separated from the main component. Therefore the solvent gradient was modified by decreasing the content of the more polar solvent (ethyl acetate) in the first step.

Second Separation Conditions:
Eluent: n-hexane with 15 / 50 / 75% ethyl acetate (%B), step gradient

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