反応 #1066200

反応方程式

4-methyl-3-nitrobenzoic acid

methanol

sulfuric acid

→

4-methoxycarbonyl-2-nitrotoluene

溶媒

water

反応条件

後処理

1. 1
   温度The resulting solution was heated
2. 2
   温度to reflux temperature
3. 3
   温度The solution was cooled
4. 4
   抽出The resulting composition was extracted with 200 ml of ether
5. 5
   洗浄The ether phase was then sequentially washed with 100 ml of water
6. 6
   乾燥The ether phase was dried over magnesium sulfate
7. 7
   ろ過filtered
8. 8
   濃縮concentrated
9. 9
   その他a rotary evaporator

実験手順

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.

出典