反应 #529838

反应方程式

NaHCO3

3,4-methylenedioxyphenylacetic acid

sulfuric acid

→

title compound

收率 86.0%

Methyl 3,4-methylenedioxyphenylacetate

收率 86.0%

溶剂

methanol

反应条件

后处理

1. 1
   温度The mixture was refluxed for 48 h
2. 2
   其他The methanol was removed in vacuo
3. 3
   萃取The residue was extracted with 1:1 hexane/EtOAc (2×100 mL)
4. 4
   洗涤The combined organic phase was washed with water, saturated NaHCO3, and brine
5. 5
   干燥dried over Na2SO4
6. 6
   其他The solvent was removed in vacuo

实验过程

To a solution of 3,4-methylenedioxyphenylacetic acid (4.2 g, 23 mmol) in methanol (50 mL) was added concentrated sulfuric acid (1.5 mL). The mixture was refluxed for 48 h, cooled to room temperature, and neutralized with saturated NaHCO3. The methanol was removed in vacuo. The residue was extracted with 1:1 hexane/EtOAc (2×100 mL). The combined organic phase was washed with water, saturated NaHCO3, and brine, and dried over Na2SO4. The solvent was removed in vacuo to yield the title compound as an oil (3.9 g, 86%). 1H NMR (CDCl3) 6.78-6.72 (m, 3H), 5.95 (s, 2H), 3.69 (s, 3H), 3.54 (s, 2H).

来源