Реакция #1563903

ord-0f088a84fcce41baaa2729bc13579dee

Уравнение реакции

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
Выход 18.9%

Реагенты

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux for 6 h
  2. 2
    ДругоеAfter reaction
  3. 3
    ДругоеThe solvent was removed
  4. 4
    workup.DISTILLATIONthe residue was purified by distillation under reduced pressure at 36° C.

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09402832B2uspto-grants-2016_08