Home Organic Chemistry Quick vacuum column chromatography: shortcut way of compound purification (VLC)
Steps
  1. 1 Prepare and pack silica gel column 00:24
  2. 2 Add sand layer and pre-wet column 01:50
  3. 3 Dissolve and load sample onto column 02:40
  4. 4 Protect column with cotton layer 03:35
  5. 5 Add mobile phase and apply vacuum 04:05
  6. 6 Collect fractions and monitor progress 05:20
  7. 7 Continue collection and verify purity 07:50
Organic Chemistry YouTube (Curated Tutorials)

Quick vacuum column chromatography: shortcut way of compound purification (VLC)

Protocol
Difficulty
intermediate

Steps

1
Prepare and pack silica gel column

Attach the flash column to a flask and pour silica gel into the column. Apply vacuum to pack the silica evenly without gaps, ensuring an even, level surface with no parabolic inclination.

▶ 00:24
2
Add sand layer and pre-wet column

Place a layer of sand on top of the packed silica gel and add a small amount of solvent to pre-wet the column before sample loading.

▶ 01:50
3
Dissolve and load sample onto column

Dissolve the crude sample in a vial using hackin and ethyl acetate, then carefully pour the dissolved sample onto the sand layer in the column. Perform a second rinse of the vial with ethyl acetate and add this to the column as well.

▶ 02:40
4
Protect column with cotton layer

Place a layer of cotton on top of the silica and sand layers to protect them from disturbance when adding the mobile phase solvent.

▶ 03:35
5
Add mobile phase and apply vacuum

Pour the solvent mixture (2% ethyl acetate in hexane) into the column as the mobile phase. Connect the vacuum line to the bottom of the flash column and turn on the vacuum pump to drive the solvent through the column.

▶ 04:05
6
Collect fractions and monitor progress

Collect approximately 500 mL fractions in separate round-bottom flasks as the solvent flows through. Perform TLC analysis on each collected fraction to identify which fractions contain the pure compound.

▶ 05:20
7
Continue collection and verify purity

Continue changing flasks and collecting new fractions while running additional solvent through the column. Check TLC results to confirm all compounds have eluted and ensure collection of pure product fractions.

▶ 07:50
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