反応 #966166

反応方程式

4-Methyl-3-nitrobenzoic acid

sulfuric acid

methanol

→

titled compound

methyl 4-methyl-3-nitrobenzoate

反応条件

後処理

1. 1
   温度the reaction mixture was heated
2. 2
   温度at reflux for 16 hours
3. 3
   濃縮The reaction mixture was concentrated under reduced pressure
4. 4
   抽出extracted with ethyl acetate
5. 5
   乾燥The obtained organic layer was dried over anhydrous sodium sulfate
6. 6
   ろ過filtered
7. 7
   濃縮the filtrate was concentrated under reduced pressure

実験手順

To a solution of 4-Methyl-3-nitrobenzoic acid (25.4 g) in methanol (300 mL) was slowly added concentrated sulfuric acid (2 mL), and then the reaction mixture was heated at reflux for 16 hours. The reaction mixture was concentrated under reduced pressure, and then the reaction mixture was neutralized with a saturated aqueous solution of sodium hydrogen carbonate, and extracted with ethyl acetate. The obtained organic layer was dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure to give the titled compound (26.9 g) as a pale yellow solid.

出典