반응 #1563903

ord-0f088a84fcce41baaa2729bc13579dee

반응 방정식

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
수율 18.9%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09402832B2uspto-grants-2016_08