- In a 500-ml round-bottomed flask carrying a dropping funnel and a connection to a condenser set for distillation, place 50 g of pinacol hydrate and 130 ml of 3 m sulphuric acid.
- Distil the mixture until the upper layer of the distillate no longer increases in volume (15-20 minutes).
- Separate the pinacolone layer from the water and return the latter to the reaction flask.
- Then add 12 ml of concentrated sulphuric acid to the water, followed by a second 50 g portion of pinacol hydrate.
- Repeat the distillation.
- Repeat the process twice more until 200 g of pinacol hydrate have been used.
- Dry the combined pinacolone fractions over magnesium sulphate and distil.
- Collect the pinacolone at 103-107 °C. The yield is 62 g (70%).
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