反応 #2275680

反応方程式

water

sulfuric acid

Malonic acid

menthol

→

dimenthyl malonate

収率 76.2%

溶媒

toluene

反応条件

後処理

1. 1
   その他is removed by azeotropic distillation
2. 2
   洗浄The organic phase is washed 3 times with water
3. 3
   乾燥is dried over sodium sulfate
4. 4
   その他The excess menthol is removed by distillation under vacuum (140° C. under 0.6 hPa)
5. 5
   workup.ADDITIONThe residue is treated with animal charcoal in isopropanol
6. 6
   温度at reflux
7. 7
   ろ過After filtering
8. 8
   洗浄rinsing

実験手順

Malonic acid (22.2 g, 0.213 mol) and menthol (70 g, 0.448 mol) are brought to reflux for 6 hours in 100 ml of toluene in the presence of 2 ml of concentrated sulfuric acid in a reactor surmounted by a Dean & Stark apparatus. The water formed is removed by azeotropic distillation. The organic phase is washed 3 times with water and is dried over sodium sulfate. The excess menthol is removed by distillation under vacuum (140° C. under 0.6 hPa). The residue is treated with animal charcoal in isopropanol at reflux. After filtering, rinsing and evaporating the solvent, 61.8 g (Yield 76%) of dimenthyl malonate are obtained in the form of a yellow oil which is used as is in the following stage.

出典