反应 #1563903

ord-0f088a84fcce41baaa2729bc13579dee

反应方程式

Oc1ccccc1O
catechol
COC(C)(C)OC
2,2-Dimethoxypropane
O=C([O-])O.[Na+]
NaHCO3
CC1(C)Oc2ccccc2O1
2,2-dimethylbenzo[d][1,3]dioxole
收率 18.9%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09402832B2uspto-grants-2016_08