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Synthesis of alpha-bromovalerophenone with bromine (large scale)

William D.

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Reaction scheme:
MjkFNdDSTO


Reagents:
Valerophenone 1 kg,
Glacial acetic acid 3 liters,
Bromine 1 kg,
Sodium hydroxide 0,5 kg,
Water.

Synthesis:
1. 1000 g of valerophenone and 3000 ml of acetic acid were mixed in the reactor.
2. Turned off stirring and left during at room temperature.
3. The pure bromine (1000 g) was neatly poured into the reactor and left in a mixture without stirring.
4. After some time, the reaction autorun occurred, severe hydrobromic acid gas leading.
5. Gas is bubbled into a mixture with absorbent (aqueous solution of sodium hydroxide, 500 g for the whole amount of water).
6. When reducing the rapid evolution of gas began stirring cautious.
7. At the end of the gas is released, with stirring, 9000 ml of pure water poured and stirring continued.
8. After 5 minutes, stirring stopped, the sediment of the bromoketone was separated from the bottom as a liquid.
9. It was separated from the aqueous layer and was re-washed with a saturated solution of soda, after clean water.
10. Used in subsequent reactions without further purification, yield: 1400 g.
 
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