反応 #1563903

反応方程式

catechol

2,2-Dimethoxypropane

NaHCO3

→

2,2-dimethylbenzo[d][1,3]dioxole

収率 18.9%

溶媒

toluene

反応条件

後処理

1. 1
   温度at reflux for 6 h
2. 2
   その他After reaction
3. 3
   その他The solvent was removed
4. 4
   workup.DISTILLATIONthe residue was purified by distillation under reduced pressure at 36° C.

実験手順

A mixture of catechol (10 g, 91 mmol), 2,2-Dimethoxypropane (8.6 g, 82.6 mmol) and p-TsOH (33 mg, 0.17 mmol) in toluene (100 ml) was stirred at reflux for 6 h. After reaction, the mixture was cooled to room temperature and NaHCO3 was added to neutralize the mixture. The solvent was removed and the residue was purified by distillation under reduced pressure at 36° C. to obtain 2,2-dimethylbenzo[d][1,3]dioxole (2.34 g, 17%) as a yellow oil. 1H NMR (CDCl3-d6) δ 1.69 (s, 6H), 6.78 (m, 4H).

出典