Reaktion #1066200

Reaktionsgleichung

4-methyl-3-nitrobenzoic acid

methanol

sulfuric acid

→

4-methoxycarbonyl-2-nitrotoluene

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe resulting solution was heated
2. 2
   Temperaturto reflux temperature
3. 3
   TemperaturThe solution was cooled
4. 4
   ExtraktionThe resulting composition was extracted with 200 ml of ether
5. 5
   WaschenThe ether phase was then sequentially washed with 100 ml of water
6. 6
   TrocknenThe ether phase was dried over magnesium sulfate
7. 7
   Filtrationfiltered
8. 8
   Einengenconcentrated
9. 9
   Sonstigea rotary evaporator

Vorschrift

Approximately 18.1 g of 4-methyl-3-nitrobenzoic acid was added to approximately 50 ml of methanol. Approximately 2 ml of concentrated sulfuric acid was added to this solution. The resulting solution was heated to reflux temperature and stirred at this temperature for 16 hours. The solution was cooled and approximately 300 ml of water was added. The resulting composition was extracted with 200 ml of ether. The ether phase was saved and the aqueous phase was discarded. The ether phase was then sequentially washed with 100 ml of water, followed by 100 ml of 10% aqueous sodium carbonate. The ether phase was dried over magnesium sulfate, filtered, and concentrated using a rotary evaporator and a water aspirator vacuum to yield 17.3 g of 4-methoxycarbonyl-2-nitrotoluene as a viscous oil.

Quelle